03-17-02 03:28
No 283684
[b]Equipment needed: Parr hydrogenator , mantle and round bottom flask with cooling column with a vent hose on top to divert gases producedinto alkaline water.[/i], buchner funnel, glass trays to dry, fan , heating lamp. Note: run your water with a pump in an ice chest with ice with an aquarium pump for the cooling column.
Material needed: - Ephedrine, or +Pseudoephedrine, chloroform, methanol,2% palladium in dark charcoal, acetone, Hydrogen gas, thionyl chloride acid
Place 200gr.of Ephedrine or pseudoephedrine in a 200ml or chloroform in the round bottom flask warm up a bit then add thionyl acid 50ml. Make sure you wear gloves and a mask because thionyl is nasty oh yes goggles because it likes moisture and it will make some nasty chocking gas.
The reaction will start one needs to only warm the flask and keep it low the reaction will run about an hour. Let it cool but make sure you take the vent on top of the cooling column now and then so no vacum is created and water is sucked into your mix.
Once the stuff is cooled put some acetone so that your product precipitates and later can be vacumm filtered with a buchner funnel using paper that will catch 10 microns. Once washed well and it is white allow it to dry very good .
Step two. dissolve in methanol just enough so it all dissolves and put in the liter bottle of your hydrogenator , once you put in your palladium in charcoal. Note vacummout your bottle first and wash twice with argon before you put in your dry palladium powder then flood with alcohol while you still have argon flowing into the bottle , as to keep the palladium and charcoal from lighting up, then add your methanol mix into the bottle , now you can hydrogenate, use all the precautions with the hydrogenator , it will take about 20-30 minutes to fully hydrogenate the solution then filter and reduce methanol in a rotovac or a crock pot till it gets syruppy then pour in a glass tray and allow to cool and crystalize use a fan and a light to blow off the excees HCl as it dries. Yu will get some beautiful crystals. The yield is about 60% of the starting material.
Note : I have herd that it can be done in one shot without the refluxing with thionyl, which is hard to get and a nasty stuff to work with. so itf anyone knows the solvent to use and catalyst for hydrogenation the lead will be appreciated.
You ask does it work................very well thank you! I hesitated posting this but I have read some good sharing from many people so I thought it was the right thing to do.
Note:
the reaction can be followed with thin layer cromatography, buy spotting starting material and a known finish product, the first reaction will spot high , starting low and finish in between using ammonium hydroxide and methanol 50-50 adjust so it does't spot too high , as your solvent and iodine crystals to develop the slides.
Good chemistry...........be safe!
(Hive Bee)
03-17-02 07:27
No 283770
What is novel about this?
What is nobel about this idea?
1 . ) Un-recycled dangerous gasses.
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Possible Phosgene formation and conversion of pseudo to meth, of course. sorry - try again :(
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(Old P2P Cook)
03-17-02 07:49
No 283772
What is novel about this?
Go shit in threads over in the Crystal Meth Forum.
This thread may actually be from someone who knows how to hydrogenate ephedrine.
(Junior Service Representative)
03-17-02 18:18
No 283902
Not that bad of a first post, IMHO; I look for to reading the followup replys...
PB
(Stranger)
03-17-02 18:20
No 283904
Well after 10 years and many barrels of E later , I know what I just gave up..........I have no knowledge of the p2p route or any other , I refined what I know.........and what do I get back .......grief! I will think twice before I contribute to this forum
(Junior Service Representative)
03-17-02 18:26
No 283906
Don't let one person piss you off that easily; where's the amounts/ratios/yields/difficulty? Any tips or tricks?
PB
(Stranger)
03-17-02 18:48
No 283909
so someone is listening and maybe interested........well the set up is explained the process is tweo parts as mentioned..
Know that thionyl chloride is very nasty with moisture so keep everything dry when you introduce it into vessel. It is best if you use a wide neclo roud bottom flask so you have a good opening for your lid for 2-3 cooling columns with proper venting for the gas produced when thionyl reacts with the solution of chloroform and E orP.
Ylu will get some reaction and it will foam up but don't be alarmed makle sure your chloroform is nice and dry from water because that's what will make it react , but with three columns that will take it and vent it out for you into the water tank with lye or sodium hydroxide.
If you go big i,e,..... 2000 gr add 2500ml ot chloroform and 400ml of thionyl the reaction will cause the solution to turn amber and wait till you see no more activity and hardly any bubles from the venting hose in the water used to neutralize the acid fumes and keep the environment safe and healthy for you and those around you .
Now no tricks up to now.............let it cool and follow with the original post make sur yuou wash well and save the used acetone , there is always some left behind so filter again in the buchner funnel.
Once dried make sure you put some aside so you can use to spot and do THC later so you can check if future batches are done right in case of problems.
Next...........Hydrogenation....need a break1
(Stranger)
03-17-02 19:25
No 283920
what phosgene? all thionyl does is make an acid chloride at the hydroxyl site , and it makes a better leaving group..........belive me that is how it works and you get a chlor.........for those of you who know the name , intermediate that in the presence of the mentioned catalyst and hydrogen , the chlorine is removed and replaced by hydrogen and whala ......meth...bye the way I read some of your replies to posts and ofcourse I wasn't able to find a single origina lpost from you, but you seem to be a sort of a censor or if it doesn't register its not possible for you to absorb.....for the lack of words. do this try it and if it doesn't work then ....give me grief........
(Junior Service Representative)
03-17-02 19:27
No 283921
Good read; keep it coming,
PB
(Stranger)
03-17-02 19:29
No 283922
I wasn't talking about soaking checken feed to extract the p2p from or put the phenyacetic acid in an aven tube to make the carbinols, but I was saying the method is clean and you need not have yellow hands from the amine stain nor deal with the yellow rim around the tub from ye yellow wet stuff that you may know how to make.......
(Stranger)
03-17-02 19:40
No 283925
You must know that thionyl chloride is watched so find something else to make the reduction to an acid chloride.
Hydrogenation:
First you must know how to use the hydrogenator , make sure you flood the bottle with argon , which is better than nitrogen because its heavier and will stay at the bottom. so while you have a small hose of argon flowing into the empty bottle witha long funnel put in your palladium catalyst and then pour some methanol to wet it then pour your mix of methanol and the material you've just finished and dried............now hydrogenate, it may take about 1200 units as the gauge goes or about 20-3- minutes i=f yuou don't poison the catalyst otherwise you will have to filter out the palladium and start again. It happens sometimes so be patient, and make sure your matedrial you just made is clean and dry.
so far no tricks straight forward............once you've filtered the catalyst out reduce in a rotovac or a crock pot until it starts forming white rim then pour in a glass tryy a nd let it cool , use a fan to blow off any gases or purt in a fume hood and scrubb the exhaust in water to keep the environment clean and your ass safe. You will get a good crop of crystals and if you are careful you may get 60+% yield .
(Old P2P Cook)
03-17-02 19:51
No 283930
and what do I get back .......grief!
Ignore Flinger, he is one of our resident psychotics.
what phosgene?
Like I said, ignore Flinger, he doesn't know anything, he just rambles on spewing random combinations of words.
The reaction of thionyl chloride with a hydroxyl does produce SO2.
(Stranger)
03-17-02 20:14
No 283933
like I said vent it into water with lye and not a scent anywhere , I use a mask with filter for the acid so to be safe , worse scenario , too much pressure and the vent gets blown off , shit all over , but don't panic just put vent back on clean up and go on , that is why you have to be there with your gloves and mask and eye wear , to protect yourself so you can cook tomorrow.......
(Stranger)
03-17-02 20:38
No 283938
As you probqlby know SO2 is a disinfectant but can be irritating to eyes and respiratory tract, that is why you wear mask for protection against So2 HCl and thionyl chloride
I found this at rhodium......its an old article , he uses ether , a bit expensive and dangerous the fumes the bust and the acetone works as well. You can see the parallel however a bit of a mix up as you will see.
Article:
../rhodium /popeye/
(Old P2P Cook)
03-17-02 22:58
No 283987
Place 200gr.of Ephedrine or pseudoephedrine in a 200ml or chloroform in the round bottom flask warm up a bit then add thionyl acid 50ml.
This is not enough thionyl chloride. Assuming that you actually mean ephedrine hydrochloride then you have 1 mole of that material but only about 80 grams or .67 mole of thionyl chloride. Perhaps this is one reason for a yield of only 60%.
(Stranger)
03-17-02 23:46
No 284004
Yes ephedrine Hcl or pseudoephedrine and you are right , I did the math wrong , namely as an example the figures were wrong , but after looking at the larger scale figures it should be 100ml, a bit extra , so to make sure in case some is lost.......
200grs of ephedrine=1.2 moles and hence need 87ml of thionyl chloride..........so for 2000grms=12moles hence need 870ml of thionyl chloride..........using it out of the liter bottle one just pours all of it just to make sure....
(Daddy)
03-20-02 17:58
No 285417
Flinger = Fman + meth = totally incomprehensible, however he is seen by us as a sort of Hive mascotte, to show the dangers of meth mis-use, and to form a treshhold for too lightly offended new members. Try to ignore witty posts, and keep posting, the balance is in giving and taking. LT/
WISDOMwillWIN
(Stranger)
03-20-02 19:37
No 285436
since thionyl chloride is watched why not just avoid that step and go straight to the hydrogenation as someone previously suggested. I can't credit anyone because no id, was on the article found on Rhodium.
I will include the whole post, however I have no knowledge of what he means as to "Everclear",or " DCM," . If anyone knows I would appreciate the heads up. I would like to see if this works. jSo here is the article:
Methamphetamine by Catalytic Hydrogenation of Ephedrine
Procedure
One 160 cubic foot tank of hydrogen was purchased for $225 dollars. A 2L heavy-walled round bottomed flask was purchased, along with a vacuum adaptor and glass stopper. Some big clear tubing with cross-hatched threads was purchased from home depot, teflon tape was wrapped aroung the threads on the H2 tank, and the tubing was just the right size so that it could be twisted and pushed onto the tank, it was sealed with some O-clamps from home depot. Using some pipe adaptors, an adaptor was made to reduce the big tube into the smaller (orange) 300 psi welding tube. The tubing was run through a standard welding pressure gage. This was connected to a t-junction fitted with hose-attachments available in the gas fittings section. One end of the t-valve was fitted with a valve, all the gass connections were aided by teflon tape and O-clamps. The 2L flask was filled with 125g Ephedrine extracted from Ma Huang, 800ml of Everclear, 10g 3% Pd/C, an egg-shaped stirbar, and 20ml of H2SO4 draincleaner. The vacuum adaptor and stopcock were attached. A clamp was placed around the flask neck, and one around the stopcock. These were both secured very tightly. The flask was assembled over a stirplate with a pot of water, which it was immersed in. The water was heated to 60C, and the flask stirred vigorously. The tube from the H2 tank was connected to the vacuum adaptor (teflon tape and O-clamp used here as well). The valve was opened and the atmosphere removed by vacuum (or mouth suction). The valve was then closed. By opening the valve on the H2 tank carefully the pressure was set to 30psi. Stirring and temp were maintained for 120 minutes. When complete the pressure was released through the valve in front of a fan blowing outside. The Pd/C was recovered by filtration. The majority of the EtOh was boiled off (~200ml remained). The 200ml of remaining reaction mix was filtered 3 times to make sure all the Pd/C was removed (you could see some was still in there). This was then dripped into 1L of 8% NaOH (premade and cooled). 125ml of DCM was added and the meth was extracted by heavy shaking for 5minutes, followed by 2 more extraction of 100ml each. The DCM extracts were collected. Dried with Sodium Sulfate. The DCM was then cooled in the freezer and bubbled with HCl gas for 30 minutes. What was recovered was 114g of clean white crystals. These were filtered and dried. The crystals were made into a saturated solution with boiling anhydrous Isopropyl Alcohol. The IPA was cooled in the freezer for 5 hours, and the snowflake crystals were recovered by filtration. Yield after this was 108g of methamphetamine*HCl (86%). And it blew the fucking pants off anything you've ever seen.
(Hive Bee)
03-20-02 20:07
No 285447
Everclear=ethanol
DCM=Dichloromethane
(Hive Bee)
03-23-02 06:16
No 286718
Hey java, what kinda fellow are ya?
has a lab with rotovap and all this...
has no problems buying thionyl chloride and other goodies...
ya very well know chemistry but try to hide this - ya don´t know DCM? Oh shit daily rotovap user pretends not to know DCM.
very funny
The demonstration of ya cut & paste capabilities was odd.
and no flames (exept TERBIUM of course..) ??????
The thread started with a description of a well known way of hydrogenation this way being completly useless to most bees as not buyable chems are used.
A obvious deep understanding of thy reaction is shown followed by pretending to have no idea of thy P2P route.
Copy & paste, copy & paste........
What are you?
indifferent feelings has
ORGY
"I hope I'm becoming more eccentric. More room, you know.
More room in the brain."
(Stranger)
03-23-02 16:37
No 286869
Very odd........your comments that is,... ten years ago many watched items were never there .......and so you stockpile, school chemistry was fun but never learned to do any practical stuff, and Methyl amine has been watched for a long time, besides my many futile attempts at synthesis through phenylacetic acid in the oven tube procedure were painful and very stinky.
If I cut and pasted someone else article , it was to be used as refrence not as a put down or an infringement on his/her time ans effort. If I 'm not familiar with some things its not a my pride only wanting to know . Yes I know the thyonil route well and if you did more research you would find that its uysed in a new type of batteries, also Phosphorous tri chloride could be substituded and its not watched , but then you knew that and was just trying to impress me with your unproductive comments and .......aren't we all trying to reach the same goal.......learn something to make something? I don't live in the states so that would indicate to you that not all governments are draconian and negate the freedom of its citizens. No insult to anyone just a comment. I try to share what I know and leave the vanity behind and ask the stupid questions, its how we learn!
(Hive Bee)
03-23-02 18:47
No 286896
Hey java,
do a quick jump over thy fence over here, yep? Look at this thread and whats ya impression?
I looked at this thread and a big question mark appeared. I wrote this post. It is not an aggressive, accusing or offending post. Is it? Did ya feel violated? If so, sorry, that wasn´t intended by me.
But to ask a question or two is thy source of knowledge and peace. Peace because if I had not asked, doubts would appear whenever I see ya name.
I´m very shure I´m not thy only doubting bee here.
For saying thy truth, I´m a lazy sack and clearing now gives me more time to do some couching (not HIVE COUCH my home couch...)
This "impress ya with unproductive comments" is mean. Hope this isn´t ya true opinion? (I behave myself, and do not rant about unproductivity & copy & paste... peace on this?)
it´s moving - but I would lie if I say I´m convinced
ORGY
not USSA habitant.
"I hope I'm becoming more eccentric. More room, you know.
More room in the brain."
edit ORGY: I did some PM´ing with java and want to state that I understand things better now. Not absolutely convinced, but not alarmed anymore.
(irritable and cranky)
03-26-02 15:11
No 288100
The second hydrogenation was from KrZ's classic write-up.
Bored...