swims journal, from epoxide to mdma.hcl

Soap · Wed Jun 01, 2005 9:39 am

well swim decided to make a journal to help any new bees (as well as him self) for these last few steps of his journey. im just here to post it for him...
any way..
Here is a picture of what he made today. he followed chromics procedure to make epoxide with 16.2 g of isosafrole:

sorry about low quality of pic, wanted it to load quickly...

That 15ml and it weighs 17.5g which is 1.17 g/ml it smells less like root beer (a lot less then safrole and iso) its a dark yellow. I plan to react it with Hcl to hydrolysis. But i can not find exact amounts of reagnts and solvents to use. only for much larger scale... heres the link to what ive found so far:

https://www.synthetikal.com/arch/forum/topic/topic_274.html

any help on the amount i should use would be fantastic.

to be continued!

Soap · Fri Jun 03, 2005 10:24 am

upon further reading it seems that practically equal amounts (by volume) of both acids (h2so4 & hcl) are used. however there is some conflicting information... is it okay to use the acid in an extreme molar excess?

heres what swim read that is confoozing him so much:

The more usual 65g batch is what most small-scale chemists do (after Shulgin, I suppose). In our case, we're just working with a mere 15g. Once you distilled out the DCM from the 250ml flask keep the glycol in and add:

25ml MeOH
120ml 15% H2SO4

15% HCl rearrangement
The extracts from a peracid rxn containing 50gm isosafrole, the glycol is added to:
75mL MeOH,
125ml H2O then
125ml 31.25% HCl.
The mixture is refluxed 2.5 hours, the oil drained from the bottom of a sep funnel and further extracted 3x60ml DCM.
The ketone distilled and at least an 80% yield can be had...

(from 29.5 g grams iso) To this was added 60 ml water, followed by 60 ml 29.5% hydrochloric acid. This mixture was refluxed for 3 hours and after letting it cool to room temperature, the dark oily precipitate was separated, and the mother liquor extracted once with 60 ml dichloromethane

so in these 3 right ups we have:

125ml 15% h2so4 for 15g epoxide

125ml 31.25% HCl. for 50gm isosafrole

60 ml 29.5% HCl for 29.5 g iso

whats going on?????

tom-a-rom-rinbow · Fri Jun 03, 2005 2:56 pm

https://www.synthetikal.com/arch/forum/topic/topic_274.html

the origional reference found highest yields with 4 moles HCl / litre of water which is 14.8% HCl.
i imagine the amount is not so important so long as you use enough and time it right.

edit: actually some HCl sitting here claims to be 37-38% with a density of 1.19g/ml. If the density is linear then 4M HCl is 1.062g/ml. so 4 moles HCl is 145.8g and 1 litre of 4M solution is 1062g. 145.8g/1062g is 13.7% HCl solution.

Soap · Sun Jun 05, 2005 9:26 am

well swim willl give it a try with 120ml 15% hcl (for 17.5 g of epoxide/glycol) what are some signs that he may be reacting to long? what happens if its reacted to long (ketone decomposition due to heat???)

anime · Mon Jun 06, 2005 4:12 am

run the reaction for 2-3 hours. (IMO 3 hours is good). You will notice the glycol turn a golden brown, golden brown droplettes will surface to the top with strong stirring. The internal temp should be around 80C. (With refluxing) Good luck with the synthesis. Have an ice bath ready to cool the reaction vessle so you do not have to wait a few hours before you can seperate the layers. There is a distinct yellow-orange aqueous layer and a brownish non-polar layer. (ketone is in this layer). IMO the extraction of the aqueous layer with DCM is not required. It does not really affect yields.

When doing the distilation of the crude ketone, make sure that the oil temp does not exceed 160C. (Please use a good vacuum source). This will minimize the amount of tar formed. This is key to getting good yields.

The tar is most easily removed when it is still hot, just pour it into something that will not melt and that you can dispose of. Otherwise a non-polar solvent is required or many washes with hot water.

Soap · Tue Jun 07, 2005 8:58 am

well swim wimped out and did the h2so4 reaction, good yeild though. but his aspirator broke while trying to distill so he freaked out and threw it back in the freezer. today he started 32.4g of iso (oxone reaction) its now t 3:30 and its a nice yellow with plenty of white particles flowing around. hes going to go ahead and do the hcl on this one for sure, cant afford to waste taht amount of ketone. Swim will check back in when hes succesfuly converted this larger amount of epoxide into ketone.

ApprenticeCook · DILLIGAF

sniff.... sniff.... so beutiful....

Nice work, keep the pictures coming, these synth documents where everything is written out step by step and pictures illustrate the words to a T are extreemly usefull to nubees and oldbees alike.

Great work again soap, have 250 points.
-AC

Soap · Wed Jun 08, 2005 9:59 am

well swim is a little worried/disapointed... his epoxide was extracted with 3x 100 ml dcm and after distillation of the dcm he only got 10 or so ml of product Evil or Very Mad

However he thinks thi shappend because he turned up the hot plate to high to get the oil heated but forgot to adjust it to keep the heat below the boiling point of the product (whatever taht is, just wanted it not to get as high as it did) any way he thinks he distilled the epoxide with the dcm so hes trying ti again. here btw is a picture of what the eopxide mixture (after oxone) should (?) look like

(blury in some parts to protect swim against big brother(they may forget this is fictional))
(this was after one wash but hte color is practiaclly the same). btw swim keeps saying epoxide and not glycol, is there an easy method to test to see what you have? and does it really matter if you do ha hot hcl hydrolysis?

Soap · Thu Jun 09, 2005 5:49 am

well the final yeald of epoxide/glycol was rather poor. swim got just about 13ml wich is about half as much as he expected... oh well on to hydrolysis... swim just added 120ml meoh 120ml dh20 and 120ml 31.25% hcl to a 500ml flask with a stir bar. he then added his 13 or so ml of epoxide/glycol (which is it!?) and started teh reaction. proably way to much acid and meoh but to much shouldnt hurt... anyway right now the oil bath is heating up (this time keeping a close eye on the temp). hopefully he will get enough ketone to run the final reaction.... (he already has about 10 or so ml of ketone...) no pics right now unless someone is dying to see waht it looks like... Confused

Soap · Thu Jun 09, 2005 6:36 am

well things are looking good, there is plenty of brown oil coming up onto the surface of the mixture, look slike the reaction will be a success. now swim is goign to have a small maount of ketone... proably around 10 or so grams, so hes thinking, use methyl mans al/hg reduction but half all reactents and use 3/4 as much solvent. still do it in a 2 liter flask and fit a baloon or condom on the stop so theres some pressure in the vessel to stop any goodies from escaping. sounds ok? swim needs to do this final reaction by tomorow night he has to give back his stirrer hot plate to his teacher....

Soap · Thu Jun 09, 2005 11:19 am

well swim is very sad. he went to distil his ketone and nothing happend. the dcm came off, he applied vacuum, the temp rose up to almost 160 and nothing came over. either he has a weak vacuum (doubt it aspirator worked fine for safroel and iso) or teh mixture si so impure ... he dosnt know. even after the three diffrent washes swims crude ketone is black. coudl this be the problem?? what are some good ways he could purify it? help this is his last day he can work on this project for a long time!!!!!!!!!

ApprenticeCook · DILLIGAF

the epoxide is an intermediate formed in the reaction with the peracid -->

The glycol is the product before acid hydrolysis to the ketone -->

Are you using MeNO2 or MeNH2 for your source?
Methylman Al/Hg is fine, take a look at osmiums variation as well, compare the various methods listed on the rhodium archive and make your selection of one or a mixture of several.
Black raw ketone? ahh should be a dirty red/brown/gold funny colour raw... then distilled ketone is usually yellow/greenish but that varies all over the shop...
Try and get a better vacuum so less heat is required.

Best of luck!
-AC

Soap · Fri Jun 10, 2005 6:27 am

well, swim fixed up his aspirator set up so its ats strong as possible.. still nothing distillling... he then tried 2 more naoh washes (throwing out the water right!!!) and still had nothing. this is his last day, and last hours with some of his more important equipment, if he cant get it to distill he may be tempted to use the ketone as is. yes yes yes he knows this coudl be a major problem but it should yeild someting right? ughhh he wishes he had more time to do this, this is a very very unhappy day fro swim... he plans to use nitromethan btw.

Soap · Fri Jun 10, 2005 8:31 am

god damn looking at that last message, swim must have been goin crazy! i have the greatest news ever! swims ketone is distilling as we speak!!! so far he has at least 7ml and plenty more to come! it only took 3 hours to get here... so what went wrong??? well first problem was the aspirator which he fixed prior to the last post. second was, get this, the oil bath was to cold! swims read multiple times to keep the bath temp under 160 so he did. well when he gave up and allowed teh temp to reach near 200... it started to boil. yes he knows that this is bad fro teh ketone but hey anythings better than what he was planiing on doing if nothing distilled. the ketone is a very clear liquid with a slight yellowish tint. absolutley beautiful. swim beleives the density of the ketone is suppose to be 1.2 g/ml so he should get around 15 or so g which is close enough to what he wanted.
So heres a question for yall: has any one ever reacted around 15g pf ketone? any advice would be great, it seems self explanitory but i know things can change drastically when the smallest adjustments are made... Will post a pic of the ketone when its done distilling. BTW if my ketone did break down because of heat it will be a dark tar right? theres no chance that what im getting could possibly be decomposed ketone right?
(pats swim on back) damn this has made my day!

Soap · Fri Jun 10, 2005 8:51 am

btw the ketone is distilling at 110 isnt that a trip??