Author Topic: trans-4-MAR synth w/o cyanogenbromide writeup!  (Read 29794 times)

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Sandman

  • Guest
Thanks moedank.
« Reply #60 on: August 22, 2003, 11:03:00 PM »
SWIM would never just go to a Lab supply w/o knowing if the wanted item would cause any concern or be suspect to the seller.

One final question: SWIM gathered about 2gm worth of PPA from the med. cabinet, but most have Chlorpheniramine maleate in them, and the largest source (1gm of PPA) has 75mg PPA with 200mg Caffeine per cap.  Would these interfere with this rxn, or could they still be used in some way?

moedank

  • Guest
I failed HS chemistry.......
« Reply #61 on: August 23, 2003, 01:02:00 AM »
I failed HS chemistry.......

I have no idea how the caffine will effect it.  Im sure Bandil can help or even Rodium so if they dont chime in I would PM one of them.

I put up a post in the stimulant forum and there is pics at the end if you want too take a look. Sorry i dont know more about chem, but im just starting out.

ONly suggestion is dont use too much sodium bicarbonate in the last step and run every reflux for as long as the OG write up says.  I couldnt believe i did it the first time. Only smell was the damn veg. oil bath.

Sandman

  • Guest
Thanks for the quick reply moedank.
« Reply #62 on: August 23, 2003, 04:33:00 AM »
Thanks for the quick reply moedank. SWIM is self educated since the 10th grade and while checking out the Hive for five years now is also only just really getting started also.  Your Stimulants forum post is what brought us here.

SWIM started a thread in that forum also Re: Prescription Stims Cost, etc. which explains the real need for help.  SWIM really thinks you've found the answer to the problem here, and is very glad you shared. Thanks!

Rhodium

  • Guest
Pure PPA, please!
« Reply #63 on: August 23, 2003, 04:51:00 AM »
You really should extract the PPA.HCl from those so that you don't have any caffeine or chlorpheniramine left, as you definitely don't want any of that to interfer with the reactions.

You should be able to find solubilities of the other substances in the Stimulants forum, as well as removal techniques, as they have been extracting pills for years...

Sandman

  • Guest
PPA Extractions
« Reply #64 on: August 23, 2003, 06:50:00 AM »
Do you think a STE backed up with an A/B would work then?

Rhodium

  • Guest
pill cleaning
« Reply #65 on: August 23, 2003, 02:09:00 PM »
I don't know exactly which pill cleaning methods removes what - Ask geezmeister.

Newbee_2Bee

  • Guest
i sent a reply (question) last night ...
« Reply #66 on: August 25, 2003, 07:46:00 AM »
what the hell happened to it? :(

Newbee_2Bee

  • Guest
Do I have the right stuff?
« Reply #67 on: August 25, 2003, 09:36:00 AM »
This (Damn Yankee) bee lives in the Southern U.S.--anybee  who is familiar knows that they are about 10 years beehind the rest of civilization!  Having an awful time finding the stuff for this synth!  KOCN...forget about it...NB2B has called every chem supply and photo supply in town - "We only sell to businesses."...checked in the major metropolis about 40 miles away...same thing.  Ok...so then I'll go the NA2CO3/urea route...I go to the 2 biggest home improvement stores in the country...one says "no urea", the other "oh yes"...now mind you, I have never bought the stuff -but am fairly sure it should be in a bottle or jar...I told the man "pure urea"...so he throws a 40lb. bag in my truck..and I get home to discover it's full of little white beads with little brown "rocks" scattered throughout!  Fertilizer for the lawn.  I remember seeing something about Cyanuric Acid--(Cilliersb-Post# 213811 says "...isn't HOCN cyanuric acid? If so, there is lots to be found at the pool store."  Rhodi replies, "I think the pool store thing is a trimer--not sure if it can be depolymerized readily."  Jim-Post#213914 says "I am positive adding water will depolymerize it"), so I assume that I can use it...and I go pick some up. 
    Here's the ironic part...all the while I HAVE the PPA...(diet pills...just like the product "DEXA-****"), capsules with little white orbs inside.  The ingredients list says "Phenylpropanolamine HCl-timed release"...that's it...no inactives!
    So now, after my 4 day shopping nightmare...I sit and read all posts in this thread and then all of them on Rhodi's site...and I am so confused I could spit wooden nickels...'cuz it seems like it's saying I CANNOT use HOCN!  Pleeeez enlighten this mixed up Bee...someone...ANYONE...SWINb2b dreamt of smoking her last bowlful of meth nearly 3 days ago...(yes-- imagined all by herself--THANKS to this and Rhodi's sites...and the input from all of her fellow bees ;) !)  To reiterate:  SWINb2b has in her posession:  PPA, Na2CO3, cyanuric acid hydrate, DH2O and 31.45% HCl.  So can I go? Or no?  :P

Vitus_Verdegast

  • Guest
well, yes
« Reply #68 on: August 25, 2003, 10:42:00 AM »
Prepare your NaOCN from urea and Na2CO3, and recrystallise three to five times (from H2O it was I believe, better UTFSE first). You want to have it very pure, with all the remaining carbonate removed.

Check the stim forum on how to extract from time-release pills, I'd guess that they probably use nasty polymeric shit for this.


Newbee_2Bee

  • Guest
The lawn fertilizer?
« Reply #69 on: August 25, 2003, 03:02:00 PM »
You mean the lawn fertilizer the guy gave me?  Cuz that's as close as I've come to urea.  So the cyanuric acid WON'T work?

Vitus_Verdegast

  • Guest
urea
« Reply #70 on: August 25, 2003, 05:43:00 PM »
Yes, urea is used as a fertilizer.

I've bought pure urea (sold for use in dye solutions, tie-dyeing etc...), that look like small white granules, resembles styrofoam but they are pretty hard.

I don't know about the cyanuric acid, but it is so simple and straightforward to make NaOCN, even a kindergarten kid could do it. So if I was you I'd stick to that.

You probably have enough urea and Na2CO3 to make 1 kg of NaOCN, which you can recrystallise many times as to obtain a very pure 99+% product.

Make sure you PPA is also very clean.


Newbee_2Bee

  • Guest
Thanx!
« Reply #71 on: August 25, 2003, 08:54:00 PM »
Thank you VV...and thanx for not flaming my A$$...I'm not a total ignoramous, just have no formal training in the wonderful world of Chemistry.  You're a Gentleman and a Scholar!  (And My...what a handsome lad, at that! ;)   I'll let you know how it turns out!

placebo

  • Guest
If one had a choice between...
« Reply #72 on: August 26, 2003, 03:21:00 AM »
If one had a choice between...

Potassium ferricyanide
Potassium ferrocyanide
Potassium thiocyanate

Which would one get?


Rhodium

  • Guest
All three are wrong, unfortunately.
« Reply #73 on: August 26, 2003, 04:04:00 AM »
All three are wrong, unfortunately. You need potassium (or possibly sodium) cyanate).

Polverone

  • Guest
the fertilizer is fine
« Reply #74 on: August 26, 2003, 11:20:00 AM »
See the little brown rocks? Pick them out by hand. You don't need much KOCN. The KOCN can be prepared more easily in higher purity than NaOCN. It's more soluble too

Post 445115

(Polverone: "More cyanate info", Methods Discourse)
. I don't know if this is important for this application, but it'd be a shame to have this procedure fail because you didn't take the time to find some potassium carbonate.

Cyanuric acid is not deopolymerized by addition to water, at least not to any significant (pH-strip detectable) extent.


moedank

  • Guest
I cant believe im reading this
« Reply #75 on: August 26, 2003, 11:03:00 PM »
PPA is the HARDEST PART!

KOCN you can order from ANYPLACE ON THE PLANET CAUSE IT IS NOT A WATCHED CHEMICAL!  It was used in the first organic synth. EVER. It is so common first year chem students will sometimes recreate the first organic synth. EVER!!!!!!

and sodium bicarbonate!!!!!!!!!!!soda ash!!!!!!!!!!come on man youre not even trying. I saw this shit on ebay for $4 a lb.  More common than dirt.  The last two chems are so easy to get, nobody is gonna even ask you shit about either one of em.  Find a big chem company, call and order the shit. USE A FCKING CREDIT CARD TOO IF YOU WANT!  Doesnt matter ONE DAMN BIT!


Sandman

  • Guest
Sodium Cyanate - interesting point Rhodium
« Reply #76 on: August 27, 2003, 11:57:00 AM »
Found this on a the Web-site of a mfg. in Japan:

"Potassium Cyanate exhibits the same chemical properties as sodium cyanate but its physical properties are different in that it has a higher solubility in water { g/100g H2O: KOCN75 (25°) - NaOCN 10.7 (16°) } and its melting point is lower. ( mp : KOCN 315° - NaOCN 550° )".

If anyone trys sodium instead, please post the results.


moedank: Sodium bicarbonate is just plain Baking Soda. Did you mean to say you found sodium carbonate on eBay? Can sodium bicarbonate even be used in this procedure?

Megatherium

  • Guest
A word of caution ... & another KOCN patent
« Reply #77 on: September 01, 2003, 06:16:00 PM »

moedank

  • Guest
yes i meant sodium carbonate. sorry bout that
« Reply #78 on: September 03, 2003, 12:39:00 AM »
That was an OK read. Id like to know how much of the product was used by the people.

Also, i dont know about the 4 to 6hour per dose shit. You do a toothpick size line of ice and you aint gonna sleep that night.  its a good 16hours per line. shit i stayed up 3days on less than a 1/4 gram. 

I saw another study on rats where they broke it down into 4 isonomers(apperenty there are 4 in ice). It was a very good read with alot of shit i didnt understand. Ill try and find it again. If i do ill post it.

Sonson

  • Guest
Now we know!
« Reply #79 on: September 06, 2003, 07:12:00 AM »
Here is some more information…and all of this is of course nothing but a dream not dreamt by me.

Cis-4-methylaminorex

To a cooled MeOH solution (50ml) of 0.025mole norephedrine freebase (3.78g) and 0.075mole NaOAc-3H20 there was added a 0.027mole CNBr in 22ml MeOH (this was made by adding 4.31g Br2 to 1.36g NaCN (97%) in MeOH) dropwise. The temperature was kept below 8°C during the addition.
The reaction mixture was the allowed to stir at the icebath for another 60mins.
The solvent was removed at the rotovap and 50ml Na2CO3 solution (sat’d) was added. The product was filtered and washed with two portions of water and dried.
The white crystals were dissolved in boiling toluene (15ml) and this solution was decanted while hot from some insolubles. Some hexane was added and the product slowly crystallized as large white plates. Mp 148.5-150. Yield 1.95g

Trans-4-methylaminorex

0.025mole norephedrine HCl (4.69g) and 0.025mole KOCN (2.09g) was added to 25ml milliQ water. Reflux for 2.5hours and the cooled in the freezer. The product was filtered and dried. Yield 4.26g.

The urea was boiled in 70ml water with 8g conc. HCl for 3h. The reaction mixture was poured into a saturated Na2CO3 solution containing some solid carbonate. This was left to stand for 2 days before it was filtered. The product was washed with water (3x20ml) and dried over magnesium perchlorate. Yield 2.1g.

The crude product was dissolved in 11ml boiling toluene and decanted while hot from some insolubles. The crystals were washed with 2x10ml petroleum ether (bp50). Mp 144-145.5. Yield 1.96g (44%)

GC/MS analysis was made on both the cis and the trans isomers on a DB-5 column (50-150°C 30°C/min then 150-320°C 15°C/min). Both were pure (99%+) with a small peak eluting shortly after the main product (at the same time in both cis and trans product.) with a very similar spectra to that of the 4-methylaminorex. The cis and trans product were separated easily, were the trans isomer eluted prior to the cis in accordance with the Cooper article in J. Forensic Chem.

Analysis of the urea in the trans synthesis proved to contain at least five different products of which the urea was present in about 45%.
The identity of the other 4 peaks is unknown.