02-25-02 16:46
No 273359
Guys, I have a few questions, and I guess some of you chemical killers can help me out.
First, I am trying to hydrolyse ergot tartrate that is 100% white, and in KOH solution continues white. I have a pharmacopeia that says ergotamine can be either white or yellow.
I am guessing the yellow one shulgin and everyone else mentions is the "other" type of ergotamine. What I want to ask is: has anyone ever worked w/ white ET? does it continue white in KOH solution? What I notice is that it turns yellow ( maybe greenish-yellow ) under UV flashes.
Well, I purify my product and I usually get a little over what I'm supposed to ( maybe 10% in average) which I find strange.
Then I proceed to the POCL3 method, I heat up, add everything, and voilá. I dry my solvent after washing and when I dissolve in methanol, I see that not EVERYTHING is dissolved. Then I add the maleic acid (20% in methanol) and very little crystalyzes. I don't get needles, but some sparse dust and I figure it's not even worth filtering.
I don;t plan to give up yet, so I dillute this whole thing in water, estimating that I have something like one gram of good LSD. I take it and I trip some. I give it to friends, and they say it's mild, but clean and the feeling is very pleasant.
My conclusion is: I DID get lsd, but why is it not crystalysing? I would like to remind that my lab is completely dark w/ blackout curtains, 20 square meters big w/ a 30000 BTU air conditioner and an extra dehumidifier, all My solvents(methanol and chloroform are HPLC, and I have an oven in which I dry all my glassware before use.
My reflux column is about -8C cold and a generous nitrogen flow (and bubbling) is present at all times in my reactions.
I have thermostats for my oil baths, the only thing I am guessing is not 100% is my vacuum pump, its giving me something like 30-40mm vacuum. Could this be so important?
I am waiting 2-3 days for drying solvents. Also, when I dry the LSD freebase, I don't get crystals, I get some sort of a plate, feels hard, but definitely is not a bunch of crystals.
Guys, help me out. I need to get some reasonable yield here.
(Oh, the ET source is pretty reliable) (and I DID get a very strong trip once, when I licked my instruments)
thanks for the time and knowledge
(Hive Bee)
02-25-02 17:49
No 273368
White is good, yellow is not so good, the collor comes from impurities. More informations thanks.
Let the malec acid/LSD solution stand in the fredge for a day ore too.
Iff you can get hold on some lyserg-something (amide,acid..) then you are home, the synthesis is not the problem. POCl3 is an 'unstabel' liquid, destilate it before use (just use a roto vap. thats fine)
You are the first person here to repoprt on an actual acid dream. If it's true you deserve a big congratulation.
(Stranger)
02-25-02 20:34
No 273386
I hope I understood something here: Im the only one tripping on my own acid? I don't believe so. What do you mean exactly by acid dream?
Also, I have a roto vap, but is it necessary to distill the POCL3? I have trouble imagining its fucked up. Ti decomposes w/ time or something? is there ways to avoid decomposition, and what are the co-products. I guess a good strategy would be to hydrolyze a lot of LSA and then distill a lot of POCL3, because to distill 2 ml at a time will cause a lot of waste, and this is not so easy to get.
Once it's distilled, for how long it's good for, considering it's in the dark, cold and dry?
Thanks a lot for your answer I never looked at the POCl3 as a possible problem.
(Chief Bee)
02-25-02 20:44
No 273390
Noone here at the Hive have written about any attempts to make LSD, ever. There are people with the knowledge, but without the needed chemicals or analytic equipment, and on the other hand there are the clueless people who believe that a synthesis of LSD is not considerably harder to pull off than one of MDMA or meth, and claim both here and there that they have made acid, when it is obvious that they don't even know what an epimerization is, or how they planned to avoid such a thing happening with their product, and how to purify the d-Lysergic acid diethylamide tartrate from epimers and decomposition products (for possible recycling).
(Hive Bee)
02-25-02 23:40
No 273425
montanha is truly a groundbreaker. So, based on your trip, what was your final estimation of yeild? can you tell us a little about your lighting setup?
heres to firsts at the hive.
oh, youasked "what is an acid dream?"
around here we dont actually carry out syntheses, we only dream of doing so. catch my drift?
02-26-02 00:50
(Rated as: insignificant)
(Moderator)
02-26-02 04:08
No 273556
As long as you don't give experimental details like volumes / concentrations / reagents and so on, we can't help you. But here are some more general remarks.
There's only one type of ergotamine. Brown colors are forming in most organic syntheses and stem from minor byproducts. Usually you don't have to care about them as long as the substance is pure enough for your needs.
You don't need dim conditions if you are working with lysergamides. I posted a paper (->TFSE) with experiments showing that light is not that harmful to LSD as always thought. They used extremly diluted solutions, if you are handling gram quantities it shouldn't matter at all...
HPLC grade does not mean anhydrous. HPLC grade solvents may have a lot of water in them and have to be dried for sensitive reactions.
If you get fresh POCl3 from a chemical supplier you don't have to redistill it. But if you are using an old and opened bottle I would definitely do it.
(Old P2P Cook)
02-26-02 04:25
No 273566
Exactly which procedure are you following? Are you following the procedure in TIHKAL?
(Stranger)
02-26-02 15:33
No 273779
Thank you for your reply. My estimated yield for LSD from
LSA was about 1g from 3.15g. I'm sure it could be better. Maybe with fresh POCl3. I'm using an very old bottle without any purification.
The room (20m^2) is completely dark with one photographic redlight. There are blackout curtains at the window and the door has a light trap made from some blackout too.
I encourage you to do your own acid as it is very satisfying. In my life I decided to trip only by my own products so I had to do it.
(Stranger)
02-26-02 15:42
No 273782
I'm trying the Shulgin method at the scale published in Tihkal. The only thing I changed on the original recipe was purifying the LSA by shaking with ether (not with the alcohol + ammonia).
I used CHCl3 HPLC which was anhydrous (<0.01% H2O). Oh, and it has some ethanol mixed to make it stable (~1%) but I think it's ok. I'm not sure about the water in MeOH (ouch) so I'll check it soon. Maybe this is why it's not crystalyzing.
I'll try soon cooking with fresh POCl3. Stay tuned.
(Old P2P Cook)
02-26-02 17:40
No 273814
For someone following the TIHKAL procedure, I would think that the 1% alcohol in the chloroform would be significant. (Assuming that this 1% is v/v) 150 ml of chloroform contains over a gram of alcohol, this could react with a significant amount of POCL3.
Is column chromatography of the LSD freebase being done?
Why is the LSD salt being prepared with maleic acid instead of tartaric?
02-27-02 01:31
(Rated as: insignificant)
(Old P2P Cook)
02-27-02 07:49
No 274104
Doing some calculations it would seem that the 1% ethanol in the chloroform is very significant. Using the TIHKAL quantities of:
150 ml chloroform
3.15 g lysergic acid hydrate (11 mmol)
3.4 g POCl3 (22 mmol)
The 150 ml of chloroform gives 1.2 gram (26 mmol) of ethanol. This is equivalent to the molar quantities of the reactants. I would guess that removing the alcohol from the chloroform would likely be much more beneficial to improving the yield than would distilling the POCl3.
(Hive Bee)
02-27-02 15:42
No 274293
Don't ever believe label claims about water content. Solvents always come wet. Especially the HPLC grade. For all water sensitive chemistry, they really need to be refluxed for ~16 hours over an appropriate drying agent like Sodium, Potassium, Sodium/Potassium Alloy (aka NaK), or Sodium/Benzophenone Ketal. THF comes so wet that you have to first distill it over LiAlH4, and then reflux!
For CHCl3, I would say to dry it with some freshly activated (still hot) 4A Molecular Sieves.
(Hive Bee)
02-28-02 10:27
No 274664
My question is where did you get the precursor? You don't have to answer that, but I wish I had your hook-ups:).
(Stranger)
02-28-02 16:57
No 274769
Terbium, thanks for the lead.
We have cleaned our CHCL3 last night (wednesday) and now we are distilling it into an ambar bottle, we will finish drying brand new LSA and in about 3 hours we will start the addition.our POCL3 is already distilled from 2 days ago, and as soon as we get beautiful needles, I will get back w/ the good news.
I am thinking if its worth it to dry the methanol first... we are very excited, and we would like to thank everyone present in the board for the attention, repplies and sincere will to help us out and hear from our success.
Really, your efforts amaze me, guys.
THANKS A LOT
(and I am REALLY sorry for those looking for ET, but I'm not supposed to mention things about sources, and mine has made this clear to me - it's a matter of loyalty)
(Newbee)
02-28-02 19:42
No 274825
If it's not too much trouble, the Hive's been waiting for a pic of recrystallized LSD for a LONG time. It would definately make a welcomed addition to every bee's photo library.
Lets see....Christopher Columbus, Charles Lindburgh, Neil Armstrong, and montanha. One for the books. Congrats.
I sell crack for the CIA
(Hive Bee)
03-01-02 20:00
No 275390
See if you can get a pic of the white light when you shake the crystals
VL_
(Stranger)
03-01-02 20:06
No 275392
Well, I have made the addition, I have dried overnight and dissolved everything. Adding the maleic acid, I got a nebulous suspension, but I don't see needles yet. Not something filterable or weightable, just the same cloudiness I got the last time...Now it's happened quicker and it's definitely a lot more crowded. I hope this crystallyzation is slow, 'cause I cannot wait to see them beautiful crystals.
I guess that if it does not crystallyze absolutely by tomorrow moring, I will add a little ether. If it does not chrystallyze at all, I will guess that the methanol is not dry and will try to determine the yields in solution.
anyone w/ any other thoughts?
(Hive Bee)
03-01-02 21:02
No 275411
[off-topic]
If you just dissolve the acid freebase in some solvent Can't you just drop it on a sugar cube or is this only possible with a solution of the salt? Can you dissolve the freebase in water?[/off-topic]
You've gotta love me.
(Stranger)
03-01-02 21:14
No 275413
I intended to start the exact same procedure (Tihkal) a few days ago but stop every thing waiting for your report.(today I began drying).
As I understand it:
In the converting of the Ergotamine to LSA part
You did not use the 15 % ammonia in Anhydrous ethanol but Et2O
You used maleic acid instead of the d-tartaric acid.
Did you use the chromatography?
Please send more details I have only 10g of ergotamine cant do any mistake
All my staff are analytical grade so with little help I believe I can make it.
I have a some lab experience.
(Newbee)
03-01-02 23:33
No 275468
From Shulgun himself:
This base was dissolved in warm, dry MeOH, using 4 mL per g of product. There was then added dry d-tartaric acid (0.232 g per g of LSD base), and the clear warm solution treated with Et2O dropwise until the cloudiness did not dispel on continued stirring. This opaqueness set to a fine crystalline suspension (this is achieved more quickly with seeding) and the solution allowed to crystallize overnight in the refrigerator. Ambient light should be severely restricted during these procedures. The product was removed by filtration, washed sparingly with cold methanol, with a cold 1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline product was lysergic acid diethylamide tartrate with two molecules of methanol of crystallization, with a mp of about 200 °C with decomposition, and weighed 3.11 g (66%). Repeated recrystallizations from methanol produced a product that became progressively less soluble, and eventually virtually insoluble, as the purity increased. A totally pure salt, when dry and when shaken in the dark, will emit small flashes of white light.
I sell crack for the CIA
(Stranger)
03-01-02 23:42
No 275473
The question was not what is written in Shulgins Tihkal but how momtanha do it ?
(Stranger)
03-02-02 14:57
No 275733
Ok, this is what's going:
1 - This is correct: I used Et2o instead of anhydrous ethanol in 15% ammonia
2 - I DID use maleic acid instead of tartaric acid
3 - I only chromatographed one trial(2nd), which was the most successful one.
I do not think this success is due to chromatography, but due to my LSA. My first LSA hydrolysis did not have satisfying results, I had a few problems w/ the temperature control and with the vacuum pump.
This last addition was made, and no crystals have formed. I guess that my methanol is NOT dry, after all.
Lilienthal, I'm sorry I didnt listen to you. I consider this now a potential cause for the crystals not to come out.
I will dry my MeOH before next procedure. Do you think CaO for a few hours is enough?
Flipper - I am pretty sure you can dissolve the freebase in water and drop it wherever you want, but one should crystallyze it to clean it and to check how much you actually have (how could this be done otherwise?)
Mosh, if you get a successful run, please get to me the details! since I can't, I don;t want to drive you off the way. What I have found is that it seems like everything should be freshly cleaned, dried and distilled, like Buzz's book says. It's really tiring to to all this, but it's not as bad as not having crystals hehehehe
If you want to know how I proceeded for crystallyzation, I only dried the solvents, added a little meoh, (not everything dissolved) then I added a little more (continued dissolving, but some didn't), and then more. Definitely w/ 4ml/gram of freebase will not dissolve the stuff... unless it has to be hot or something...or it takes a hell of a long time. Well, after (almost) everything was in solution ( some stubborn crystals appeared I don't know where from) I added the MeOH (20% maleic acid sol.) and the mixture turned rather quickly into a cloudy mess. Only problem is it continues to be a cloudy mess. I am not sure, but I added some old LSA to complete 3.15 grams, and the solution turned dark in the last 6 hours. The first attempt resulted in a very dark solution also, w/ apparently lower yields. I am guessing that some ET went in there (either ET or other impurities). I still have a few attempts before I cry, I will definitely chromatograph every run from now on.
(Stranger)
03-02-02 15:31
No 275741
Thank you for your replay
My Methanol is 0.03% water.Is it dry enough?
The Ether is dry 0.0075%.
My biggest concern is the dry ammonia because I can;t use pure ammonia where I work
Did you warmed the MeOH?
(Stranger)
03-04-02 21:30
No 276814
If these labels tell the truth, I guess your solvents are dry enough.
I am told, though, by a bee, not to trust them.
I have a surprise for all of you. I am very shocked!
I washed my chloroform in nh4oh and then dried it. I am a very lazy person, so I left a tiny little bit of chcl3 in the 2L sep funnel and dried the rest ( which I dilluted in the WARM methanol and then added maleic acid). This didn't give me many crystals yet - maybe the methanol is NOT dry.
Dilluting it in 400ml water, I see that one drop is a fine hit, though. meaning I got this time about 8000 hits. this is fine, I started out from 2.5 grams this time. now I DO have a big surprise. I need expert advidse for this one.
TODAY I was going to wash the sep funnel w/ nh4oh (and the little bit of chcl3) and I noticed a reasonable ammount of STAR-SHAPED CRYSTALS that formed in the funnel! they weighed .4 grams and they have a blue fluorescence!!!!!
I AM DYING TO TRY THEM TONIGHT!
I will dillute it and tomorrow I will come tell you guys what happened.
Might this be freebase crystals? maybe the CHCl3 evaporated and the nh4oh made the Slow crystallyzation form those beautiful stars ( which later, broke into tiny needles)
I would love answers before I take these.
If I don't get them, I will take them anyways. I don't want to wait a week to analyze this. I "bee" too anxious too wait hehehe...
Later
(Hive Bee)
03-05-02 17:50
No 277225
like you said, might as well try to dry out the methanol. You have no reason not to.
heheh, oh and i hope you didnt fry yourself...you havent updated us for a while. ( the fear and loathing bathtub scene comes into mind.)
(Stranger)
03-05-02 18:17
No 277240
any news on bioassy?
-herb
(Stranger)
03-05-02 21:19
No 277314
actually, I do have some news.
My darn methanol finally showed something.
In the last 30 hours the clowdy mess turned into thicker balls of crystals! Tey're definitely not needles, but it is now clear that something has formed. and it looks like it's more than one gram. I haven't weighed it yet.
I wonder why it took so long.... and I do hope its my product. I will wait another day to see if I get more and I will filter ahd weight tomorrow.
THEN I will try it. What should I do if it works? send samples?! take pictures? jump 2 meters?
(Stranger)
03-05-02 22:09
No 277331
Please send your full procedure.Colors, weights, time,temperature etc.
I began today and the first thing I noticed is that the Color didn;t change to yellow Even after the 4 hours in
75°C with nitrogen bubbled into the stuff. The color is light brown.
My ergotamine was white.
(Chief Bee)
03-06-02 00:36
No 277401
Do NOT forget to post pictures of your LSD crystals! We want to see a pile of crystals that's enough for a few thousand hits...
(Stranger)
03-06-02 16:11
No 277847
Right
I will post the pictures. But I am doing quite a few hydrolysis before I do the next step. I feel that this will save me a lot of time, since I will do an entire clean procedure w/ all fresh materials and all.
when I am going to have good looking crystals I will definitely take pictures of'em. About the procedure... I can take pics of those, but I have to fix a nice lab setup ( my lab looks like shit! ahaha)
see, I'm shy.
but I'll do an effort and I will photograph the procedure.
Mosh is right, The ET does not go yellow in solution, mine remains white and very clear. It's color changes under UV, though. I will try to show these differences.
I'm scared someone might trace me back though.
Rhodium, you mentioned purification of the LSD tartrate from epimers and decomposition products. Is there a further way to purify the LSD other than packed column chromatography?(of course there is, but not using 200 thousand dollars equipment) (THE COLUMN WILL LOOK GREAT ON THE PICTURE ALBUM!)
and what would YOUR plan be to avoid the darned epimerization of the alpha-carbon from happening during reaction?
(Stranger)
03-06-02 17:07
No 277878
Can you send written procedure mainly about the ergptamine ==> d-lysergic acid hydrate procedure?
I am very confused about skipping the ammonical ethanol part.
(Stranger)
03-06-02 20:07
No 277948
please publish instead of pm, this is of utmost interrest
-herb
(Chief Bee)
03-06-02 20:14
No 277952
I don't recall exactly where the information is located, but I know that among the LSD synthesis documents at my page, there are instructions for minimizing epimerization and how to convert iso-LSD to LSD. Column chromatography is the way to go for purification.
(Hive Bee)
03-07-02 01:11
No 278054
"Convert iso-LSD to LSD. Add 50 ml of ethanol and 5 ml of 4 N KOH per every gram of iso-LSD. Let this mixture stand for 2 hours at room temp. Evaporate in vacuo to get the LSD.
Separate iso-LSD from LSD. Dissolve the residue of the mixture of LSDs from the end of the formula in 120 ml of benzene and 40 ml of chloroform. Add tartaric or maleic acid to precipitate the LSD, filter off, add a little ether and put in refrigerator for several days to get a little more LSD, which is filtered off and added to the rest. Evaporate the filtrate in vacuo to get the iso-LSD and convert as above."
above excerpt from ../rhodium /lsd-buz
(Hive Bee)
03-07-02 02:05
No 278081
http://jaxindy.chem.yale.edu/
maybe that can help. i cant find much on lessening epimerization on rhodiums site. maybe im just blind, but are you sure theres something like that there rhod?
(Chief Bee)
03-07-02 03:03
No 278109
From the same document as above:
LSD From Lysergic Acid Monohydrate
This is, in my opinion, the best of all the methods. It was designed to be used to experiment with different types of amines, so if you would like to substitute diethylamine with another amine this would be the best bet. It also gives good yields (50% or better) and is very easy. The reference that gives it also gives potency data for many lysergamides and many of their formulas. The reading is good, interesting, informative, and the method given below gives no useful amount of iso-LSD, so separation of that product is not necessary. Both method A and B were from JMC 16, 532.
It was several months ago I last read the documents, so my recollection of the contents was not entirely correct. There were no discussion about how to minimize epimerization other than the above - a note on which method to use. Either my site is becoming too large, or my memory is failing - I can no longer memorize all its contents.
(Stranger)
03-08-02 01:25
No 278628
any news ??
(Chief Bee)
03-09-02 20:47
No 279642
Epimerization Studies of LSD using 1H Nuclear Magnetic Resonance (NMR) Spectroscopy
S.J. Salamone, Z. Li, A.J. McNally, S. Vitone, and R. Wu
A study was conducted to determine the conditions needed to achieve the equilibrium concentration for the epimerization of d-lysergic acid diethylamide (LSD) to iso-LSD. The reaction was followed by integration of the C-9 resonance of LSD and iso-LSD by proton nuclear magnetic resonance (NMR). The C-9 resonance of LSD and iso-LSD appear as singlets at 6.35 and 6.27 ppm respectively. Starting with pure LSD, the conversion to iso-LSD is attained at temperatures above 37°C and pH levels over 7.0. At a pH of 7.0 or higher, the LSD/iso-LSD ratio of 9:1 is achieved after one week at 45°C or two weeks at 37°C. Starting with iso-LSD, the conversion to LSD requires more vigorous conditions. The 9:1 LSD/iso-LSD ratio is attained only after 6 weeks at a temperature of 45°C and a pH of 9.7. At lower pH levels, the reaction proceeds more slowly. The 9:1 LSD/iso-LSD ratio is achieved whether the starting material is LSD or iso-LSD and therefore represents an equilibrium concentration (K = 9). In addition, the more vigorous conditions needed to achieve equilibrium of iso-LSD to LSD demonstrate the difficulty in extraction of the epimerizable proton of iso-LSD. This study is the first to quantitate the epimerization of LSD by NMR techniques and establishes the conditions needed to induce epimerization in solution.
Ref: Journal of Analytical Toxicology, Volume 21, Number 6, October 1997, pp. 492–497.
(Hive Bee)
03-11-02 00:11
No 280260
any news montanha?
(Hive Bee)
03-11-02 03:14
No 280350
You didn't spill it on yourself or something, did you?
I sell crack for the CIA
(Hive Bee)
03-11-02 05:36
No 280411
God damn it he probably did spill the damn shit it on himself. this is how come there is no fucking acid in this world. as soon as someone new learns how to make it they damn spill it on themselves and fuck it up for the rest of us. Did he not realize that the whole country was depending on him.
VL_
(Junior Service Representative)
03-11-02 05:50
No 280424
LMAO!
PB
(Stranger)
03-11-02 20:41
No 280720
Hi guys,
I'm still alive. I didn't spill it on myself. Well, I did but am still very alive. In the last few days I worked very hard to hydrolize a few more grams of ET (100g) and now it's time to do the same with some ergocristine I had floating around (hehe, that's another 50g -- I love my source). Then I will carry more consistent experiments about dietilamination (!?). Keep tuned. I'll picture my procedures in a few days to satisfy your thirst.
I left a beacker in the freezer for crystalization some days ago and today, WOW, I had a marvelous vision: lots of crystals!
See you soon,
Montanha's partner (aka Stilldonthaveanickname).
(Junior Service Representative)
03-11-02 21:43
No 280761
Just PM me if you need a willing guinea pig to confirm the activity of these crystals...
(In my dreams, perhaps one day
),PB
(Hive Bee)
03-12-02 04:24
No 280951
Oh, sure, my spare 100g of ET. My spare 100g! You self-riteous motherfucker. I mean, uh... Good work dude, we're all....proud of you. Yeah. Really fuckin' proud. Unintelligeble grumble.....
Just kiddin' dude.
Tell me something, though. Is the recrystallized LSD in one bug crystal, or just a lot of crystals layin' on the bottom of the beaker?I sell crack for the CIA
(Stranger)
03-13-02 01:37
No 281558
El Zorro, thanks for the compliments!
and as for your question, through my reading of a few references and procedures, I thought I would get needles, like the oxime when I make MDA. they form big, pointy and even hard needles - really beautiful. What I got from the LSD is a bunch of crystals lying in the bottom of the beaker
To be honest they don't look so good. I didn't dry them totally yet, I am waiting to make sure they don't grow any bigger. When I dry them, I will definitely shake them. maybe record this and post it if it looks good.
I am trying, though, to take nice pics of the setups, but I will definitely need a decent UV light to show the column during chromatography, the crystals glowing and all that. I have a small, handheld UV I bought from this piercer dude that shows everyone his glow pierces, heheeheh.
no, I don't use piercing.
I guess I will start my procedures again and filter what I have to dry, shake and try...
Later, people
(Hive Bee)
03-13-02 03:14
No 281612
No prob, dude!
I did have one thing about the Shulgin synth(or the workup, rather,) that I never quite understood. He says that when he was recrystallizing the finished product, he says he did repeated recrystallizations from methanol, and the product became increasingly less soluble. Does he mean he just heated some up in methanol, and filtered out what didn't diddolve? How does he know that this doesn't have impurities? And so does this mean that your final product is the filtered material?
I sell crack for the CIA
(Old P2P Cook)
03-13-02 07:34
No 281812
He says that when he was recrystallizing the finished product, he says he did repeated recrystallizations from methanol, and the product became increasingly less soluble.
Yes, that was a very interesting statement. I wish he had elaborated.
(Hive Bee)
03-13-02 21:13
No 282069
Someone needs to get in contact with Shulgin and convince him to join the hive and helpl support our cause. He definatly is a supporter of the cause. His expertise would be very wonderful here. About 1/10 of the questions here are in refrence to his work. Mabyee he already is.
VL_
(Distinctive Doe)
03-13-02 23:42
No 282101
I think used to bee.
Some thought Rathead(i think) was possibly Shulgin.
Those who give up essential liberties for temporary safety deserve neither liberty nor safety
(Hive Bee)
03-14-02 00:48
No 282138
I bet he's sittin' back and readin' this shit right now! Hey! I see you there, Shulgin!......Hey! Where are you goin'!?! Come back!......I'm gonna catch you motherfucker!
I think We're all just foaming at the mouth just waiting for those pics. Maybe even a 15 sec. mpeg of the flashes of light when the crystals are shaken.
Another thing, how do you know the solution stays white if you're working in red light conditions?
I sell crack for the CIA
(Stranger)
03-15-02 00:11
No 282665
OKeyDOkey!!
I am getting better at this!
I guess all the solvents and reagents we buy are shit. Success seems to increase when you clean up reagents and solvents.
nothing can now be fucking up my reactions.
As to your question, El Zorro, I DO turn the regular light on for moments to see the reaction, how it's going and everything.
Does anyone know how to purify dietilamine?
Thank you all,
Montanha
(Master Whacker)
03-15-02 04:23
No 282767
No doubt about it, simple distillation at STP with a crude column is all that's needed for purifying diethylamine. Pure diethylamine is water white and that's what you will have after distillation. After it sits around for a while it turns yellow indicating need for redistillation. (Someone used to like DET a lot around here!)
(Junior Service Representative)
03-15-02 05:17
No 282792
Wasup wit de pictures?
PB
The Hive lit my fuse, now watch me blow up!!!
(Hive Addict)
03-15-02 22:24
No 283091
He probably spilled it on himself again and this time it was way concentrated due to his improved yeilds. If he is Okay and anyone knows him personaly then give him a biosuit. this man needs to stay sane.
VL_
(Hive Bee)
03-15-02 23:23
No 283117
He was probly workin' along, then some got under his glove. Next thing ya know, he saw a bunch of penguins trying to break his glassware! So naturally he called animal control, and told them the whole story. Where is our poor montanha now? Why, I'm sure you all can guess!
But seriously, though, if you have 100g of ET layin' around, have you considered using other peptide coupling agents? Post 122826 (dormouse: "new routes from ET to LSD -pHas3d", Serious Chemistry)
I sell crack for the CIA
03-16-02 03:48
(Rated as: insignificant)
03-16-02 12:25
(Rated as: insignificant)
03-16-02 19:31
(Rated as: insignificant)
03-17-02 00:15
(Rated as: insignificant)
03-17-02 09:14
(Rated as: insignificant)
(Hive Bee)
03-18-02 00:26
No 284017
Dear Montanha :
My knowledge of chemistry is not that much, but I know something a friend told me about POCl3 that I decided it was worth posting :
I friend of mine once told me he knew someone who was a semiconductor technician, he died of lung cancer, they believe a main factor was the fact that he was allways working with POCl3 and not taking the adequate precautions.
I recomend you to avoid skin exposure or breathing the vapours of POCl3. Since all I have is word of mouth, even being it from someone I trust, I would like someone else to confirm this if possible.
(Junior Service Representative)
03-18-02 01:41
No 284048
Toxic substance: http://www.sci.ccny.cuny.edu/~tbandosz/E
And this said not classified by the NTP for cancer: http://atsdr1.atsdr.cdc.gov%3A8080/gsql/
PB
(Chief Bee)
03-18-02 02:32
No 284087
If you are making LSD with the POCl3, you will only have to use it at most once a year or so, considering the potency of LSD. That shouldn't be a health problem.
(Hive Bee)
03-18-02 03:08
No 284105
Personally I have no interest in this synthesis, I have dropped acid some 10 times or so, many years ago, I no longer use it.
My friend might have jumped to a wrong conclusion, I have done a fast search on ChemFinder and on the WWW, I got one list of carcinogenic substances, POCl3 was not listed there.
It is mentioned as quite toxic, in agreement with what PoohBear4ever has posted. I should have verified things more carefully before posting, please excuse me.
03-21-02 04:13
(Rated as: insignificant)
03-21-02 19:39
(Rated as: insignificant)
(Stranger)
03-22-02 02:28
No 286119
Alright all you happy bees!!!!
I'm BACK!!
I have taken a week out of town, and I am getting back to work now!!!!
I would like to thank you all greatfully for all the repplies, support and concern - NOT TO MENTION KNOWLEDGE!
I feel like jumping out of my skin when I read posts comming from you guys!
I have made, like I stated, quite a bit of LSA. I will now do the next step several times, too. I DO have one thing I didn't mention. Just before I took a break, I dried a certain ammount of LSA cause I thought I would work on it right away. Anyways, I heated it up to 130C and vacuumed its atmosphere. after 3 hours it became grey.
This is the first time this ever happens.
I was worried to have burned out some of it ( which was one of the reasons I decided to rest) but when I cabe back, there it was! nice and white again!! Weird? maybe the LSA hydrate is white, and monohydrate grey. Does this make any sense?
well, I will try to work on it grey from now on. Maybe it improves the yiels. If it does not work, I won't heat it so much anymore.
And I WILL come back with pics soon, I promise to get the next step in detail. Then I will pic the hydrolysis of my cristine.
Later, guys!!! Don't forget to write!
(Hive Bee)
03-22-02 02:41
No 286126
WHy are you drying it? The Shulgin(yeah, you, Shulgy, I know you can hear me!) synth uses the hydrate, doesn't it? Lemme check....yup, sure does. But if you were going to dry it, why would you heat it up to 130°? I would be afraid of damaging the precious LSA. Couldn't you just dissolve it in anhydrous methanol, then add drying salts, then rotovap off the methanol under dry nitrogen or argon? I would think that that would be a lot more gentle.
I still think the Hive could greatly benefeit from research into other coupling agents. But for now, I'd just be happy with a couple pics.
I sell crack for the CIA
03-22-02 02:47
(Rated as: insignificant)
03-22-02 09:36
(Rated as: insignificant)
(Hive Bee)
03-23-02 02:45
No 286656
You're killin' us man! Where's the pics at??
I sell crack for the CIA
03-23-02 05:50
(Rated as: insignificant)
03-23-02 10:12
(Rated as: insignificant)
03-23-02 10:36
(Rated as: insignificant)
(Stranger)
03-25-02 15:02
No 287626
guys, montanha is now very sad.
Montanha wants to say something about LSA.
LSA, when filtered, is not a dry powder. it is more like a paste, and it has to be dried, or one won't even know yields (20 grams, out of the filter cake comes to 3 or 4 grams dried). This is why montanha dries it. Montanha decided to get all the water out a while ago and noticed it turned grey. Today, montanha added it to the CHCl3 Solution and it turned BLACK.
Montanha guesses it burned out!!!!!
part of it dissolved, so I continued with the POCL3 addition, but I have no more hopes of getting good ( if any) crystals with this run.
Problem is, Montanha wished he could add DEA to all his ALREADY DRIED AND PROBABLY BURNED LSA.
Montanha really thinks he fucked it up this time. Montanha was even ready to take pictures for his brother bees at the hive.
Montanha needs help.
This is worse than a bad trip...
The solution did turn amber, though, so maybe there is a little bit of good stuff in there.
Montanha hopes he can get it out.
Word of advice: never overdry your LSA.
(Hive Bee)
03-25-02 15:20
No 287630
An easy way to dry a powder is to disolve it into some solvent (ether,toluene,DCM aso.) then dry the solution with MgSO4, filter the MgSO4 off and evaporate the solvent off, you now have a dry powder.
Bac to problems, what were you dooing ??
I dont think tha disolving LSA into CHCl3 will harm it at all, My guess is that you have some kind of (black :) contamination in your LSA, try to filter the CHCl3 solution trough 3-4cm kiselgel 60 (or some other collum powder) Usual the black tarr stick to the kiselgel.
(Hive Addict)
03-25-02 19:01
No 287687
I wonder why you think you can only dry things by heating them. If you have access to things like POCl3 and so on, you probably also have a vacuum setup somewhere. Just dry your LSA with vacuum. Only watch out that your LSA is not too wet; otherwise you'll have LSA all over the place.
BTW, there's also a lot of discussion of drying techniques in Vogel. So this is probably a fuckup that you could have prevented...
(Hive Bee)
03-25-02 19:38
No 287697
RE Montanha decided to get all the water out a while ago and noticed it turned grey
Was it heated or exposed to light?
What drying method did you use?
In the future, after filtering the LSA remove the filter cake and place it in a watch glass. Place the watch glass in a vacuum dessicator, or a bell jar, overnight (cover the dissector, or bell jar, with tinfoil to prevent light from entering). Depending on how strong your vacuum source is, the cake should be totally dry in the morning. This would probably work very well considering the fragility of LSA.
Sorry to hear about the burned LSA that must hurt.
The Ultimate Weapon Can't be controlled, banned or confiscated. Your weapon's your mind.
(Hive Bee)
03-25-02 22:05
No 287746
I don't think your problem was overdrying, I think it was the whole 130°C bit. I think you probably burned it. Shulgin said that he just dried it under vacuum to a constant weight, he didn't say anything about heating it.
I sell crack for the CIA
(Hive Bee)
03-26-02 19:59
No 288165
I heated it up to 130C and vacuumed its atmosphere
I didn't read that.
You can't get LSA that hot. That was your problem. You might be able to salvage some of your product. But most of it is probably destroyed.
The Ultimate Weapon Can't be controlled, banned or confiscated. Your weapon's your mind.
(Chief Bee)
03-26-02 20:14
No 288173
Please Mr Montana, could you write a DETAILED description of what LSD synthesis you are trying to perform (with times, temps, reagents), and give us the batch size, your equipment (what do you have - mp apparatus, rotavap, TLC analytical equipment?), solvent grades, and which salt you are planning to form of the LSD?
Please do that, and we will all try to give you as detailed suggestions as possible for you to to perform this feat successfully with as high yield humanely possible.
My little heart aches when I read about burned precursors, of a kind that I will never be able to get. I just feel that I could have done so much nice things with the little fragile molecules which now are nothing but a memory and a little grey puff of smoke...
(Hive Bee)
03-27-02 00:44
No 288289
I read in an article the Rolling Stone did about some famous acid chemist that his first batch turned out black. From what I recall, he was very distressed by this but it turned out to still be active.
You aren't giving up, are you?
Better loving through chemistry.
(Chief Bee)
03-27-02 00:51
No 288292
Color is not of any importance as the product must be column chromatographed just before crystallization anyway. The only thing it means is that the yield will be a little lower.
(Stranger)
03-27-02 03:50
No 288355
A quick question for you rhodium. I searched and came out inconclusive. How high of a risk am I at with the the double bond between the carboxamide attachment and the aromatic ring forming lumi-LSD. Some is dissolved in EtoH, and some remains in crystal form in an amber bottle. I would like to take some pictures for you all but am scared of decomposing my LSD. What conditions do you suppose I take the pictrures in? All I have is a digital camera. Should I turn the lights on? Under red light? Leave the flash on? I guess the question Im asking is what conditions are best with less chance of degrading, but still get a good enough picture?
(Hive Bee)
03-27-02 04:34
No 288377
A quick flash or two will do little if any noticeable harm
. The Ultimate Weapon Can't be controlled, banned or confiscated. Your weapon's your mind.
(Hive Bee)
03-27-02 10:27
No 288467
Afaik. LSD is not that unstabel, usual it's not the light who 'kill' it but Cl- ions from the wather (or the blu ink at the blotter :)
(Hive Bee)
03-28-02 00:40
No 288723
Hey rhod, ever dredge up any info on lsd epimerization?
My computer was hacked by whatsupium!
(Chief Bee)
03-28-02 01:06
No 288742
Bujinkan: Only what I posted in Post 278109 (Rhodium: "Re: trouble getting yields for LSD", Tryptamine Chemistry) - all the LSD info I have handy is already online.
04-01-02 06:51
(Rated as: insignificant)
(Newbee)
04-04-02 05:53
No 292142
It must really suck fckin up the best drug in my known world. But hey just relax smoke a fatty and try again.
From what I've read LSA decomposes at 238 degrees. Also it supposedly forms hexagonal leaflets when crystalized. From what I've read it should be dried at 140 degrees at 2 mm HG. But I don't know if this correct. Also, you people make the production of ergot alkaloids seem to be as hard as making an atom bomb. Don't get me wrong, it is definatley not even close to easy. But they can always be bought, if your willing to pay enough and are to lazy to try real hard to make em. I was told that i could get a gram of ergotamine tartrate for 600 a gram and i found some bromocryptine for a little less. This obviously was way to expensive though. I still know of some other options which could signifigantly reduce the price but i haven't (and probably won't) look into such things (well maybe i will in a dream or something). If you think really hard, than you can figure out where to buy it, but when buying it be prepared to pay a hefty sum of money. This seems to leave all of us poor people who can't afford to wipe our asses with 100 dollar bills in the shitter. Therefore your just going to have to make it, and if you can get as far as the alkaloids, but no further, than still make em and just sell it to someone who can. There never seems to be enough acid around, and maybe if people made this into a larger operation than just a one man job then something might really be done. But i'm just rambling. Don't even fuck with goin around inocculating fields of grain, or looking for those little kernals all damn day when your sure not to find as much as you need. The only feasable way it seems to me is to grow just the culture and then to extract the alkaloids from there (don't forget to defat). Sure this isn't easy, but it takes being a damn hillbilly farmer out of the picture as well as the need for land, a tractor, and all that other BS need to grow the grain you plan to infest. The easiest recipe i have found for the medium needed to grow the culture consisted of 20% Cane Sugar, 3% peptone and water (it said tap, but where i live i don't feel safe bathing in tap). Then you just the PH to 6.2 with ammonia and incubate at 24 degrees for 8 to 10 days. And voila you have like 1 to 1 1/2 grams of ergotamine per liter of substrate. I would suggest fcking around with cubies first so you can get the hang of growin cultures a little better. I'm sure this has been posted before so don't even bother with the UTFSE, cause i'm not gonna come back to this thread. But please if you make some fry in your dream, make alot and attempt to Pyschadelisize (i can't spell) the US, cause I'm tired of looking for acid,i wish it would just fall out of the sky while i was tasting a rain drop. Wow wouldn't acid rain be cool. But don't forget, smoke a fatty and keep on truckin.
_.-==''SupaTokaBuDsMoka''==-._
'''''''GonnaGetHighTillIDie'''''''
(Hive Addict)
04-07-02 13:25
No 293631
Hey mottaman...many mistakes must be made before perfection...dont give up.
and to montanha, keep going. Dont stop. The hive is your support completely!
(Stranger)
04-07-02 17:52
No 293708
alright, I got some new ET ( which later I found out to be dihidro something ergocristine masilate, which I think will be the same thing)I have hydrolysed 10 grams, and am waiting to get ammoniacal ethanol solution and clean it ala shulgin. this time I will follow exactly all his steps to repeat his yield and crystallyzation. I want to get this completely right for once and move on to research some about BOP or HBTU coupling, to make my contribution to the HIVE. Once Iget this procedure going ok I promise to send pictures
later, guys
(Moderator)
04-07-02 18:48
No 293719
Yes, it's a good idea to stick with the inactive and not controlled stuff to learn the procedure
. BTW, I perfectly understand that all of you you like to swank about syntheses you never made. But it would help a lot it you could make it bit more obvious. Otherwise you are risking to be banned because of not following the rules (https://www.the-hive.ws).
04-11-02 08:00
(Rated as: insignificant)
(Hive Addict)
04-15-02 18:47
No 297223
something ive always been curious about is decay rates of LSD from light, oxygen, other environmentals. Montanha, did you continue to use extremely diffuse light on your subseuent attempts? do you have any other observations on molecular decay to share with us?
btw, you are my personal hero.
blow me down! -captain morgan and the straw house
(Chief Bee)
04-17-02 02:01
No 297855
(Rated as: excellent)
Stability Study of LSD Under Various Storage Conditions
A controlled study was undertaken to determine the stability of LSD in pooled urine samples. The concentrations of LSD in urine samples were followed over time at various temperatures, in different types of storage containers, at various exposures to different wavelengths of light, and at varying pH values. LSD concentrations were measured quantitatively by the Abuscreen RIA and by HPLC using a fluorescence detection method. Good correlation was observed between the immunoassay and the fluorescent integrity of the LSD molecule. Thermostability studies were conducted in the dark with various containers. These studies demonstrated no significant loss in LSD concentration at 25¡C for up to 4 weeks. After 4 weeks of incubation, a 30% loss in LSD concentration at 37¡C and up to a 40% at 45¡C were observed. Urine fortified with LSD and stored in amber glass or nontransparent polyethylene containers showed no change in concentration under any light conditions. Stability of LSD in transparent containers under light was dependent on the distance between the light source and the samples, the wavelength of light, exposure time, and the intensity of light. After prolonged exposure to heat in alkaline pH conditions, 10 to 15% of the parent LSD epimerized to iso-LSD. Under acidic conditions, less than 5% of the LSD was converted to iso-LSD. We also demonstrated that trace amounts of metal ions in buffer or urine could catalyze the decomposition of LSD and that this process can be avoided by the addition of EDTA. This study demonstrates the importance of proper storage conditions of LSD in urine in order to insure proper analytical testing results over time.
Ref: Journal of Analytical Toxicology, Volume 22, Number 6, pp 520-525 (1998)
(Stranger)
04-19-02 15:14
No 299084
It has been my experience, that any reagent can be acquired. With a little effort and creativity, almost anything can be purchased outright. Those items which are super "Hot" can be produced if needed. If the members of this forum are really interested in LA, they will find a way to produce it by culture, extraction, or synthesis. And, they will find a way to produce a lot of it. Access to the hive mind, allows hundreds of years of experience to be focused on solving a problem. Dead end research is avoided. What used to take a chemist years to ferret or experiment out, is gladly gifted within minutes. In this arena, to say you will never have a reagent, or be able to run a reaction, isn't quite accurate. You will be able to do, whatever you wish to do. Each of us has different goals, and each of us has a different role to play in life. And, each of us knows that there is a price a pay to achieve a goal. For some reason, perhaps it is the will of god, it seems important that these products be produced. It is not required for everyone to actually produce them. For those that actually make the honey, there is a price to pay. The tip of the pen, does the hardest part of the job, that is where all the pressure is. Each of us, can make as much LSD as we wish to. The world only requires that a few of us make that sacrifice.
Here, with help, a relative novice is rapidly becoming a master craftsman. This is good. The question is: can he or she, avoid the snares of the world, maintain invisability, and avoid harm? Excaliber was the greatest of swords, but its sheath was greater. As long as Arthur wore it's sheath, he could not be wounded. [center]
Now, the important lessons, are in survival.
(One Man Show)
05-01-02 23:03
No 303914
I would be interested to know how much LSD floating around (and there is none where I am) was salted with maleic. I assume this was done to help reduce oxidation potential.
"Have we descended to the level of dumb beasts?" Fear & Loathing
Be loved and blessed hp and cg!!