trans-4-MAR synth w/o cyanogenbromide writeup!

[Vibrating_Lights]

WHere is the ref for PPA with nitroethane/benzaldehyde.  Also Can KOCN be found over the counter.  or can it be generates from potassiumferrocyanate

[Prometheuz]

KOCN is non-toxic and not a suspect chemical to order. If you can buy basic chemicals somewhere, you should have no problem getting KOCN. It's cheap as well.  

[Rhodium]

WHere is the ref for PPA with nitroethane/benzaldehyde

Search for posts by Barium. He has made several substituted PPA's recently.

[Vibrating_Lights]

an you be a little more specific about where to look for the ppa from nitroethane patents. I cant sem to find them.
vl_

[starlight]

Patent US2151517

[Wouter]

Bandil wrote: SWIM was of course VERY thrilled when the white stuff precipated as an amide would not have done this ...

If the amide wouldn't precipated, will this means when you use a mixture of norephedrine and norpseudoephedrine, that you can easily separate the formed amine from the amide?!?! Instead the VERY DIFFICULT separation of norephedrine from norpseudoephedrine before.

[Rhodium]

Yes.

[moedank]

Swim followed this synth. to the letter and everything went fine.  Swim only did a small bit and has been up since thursday!  Couple foils every now and then .  Way better than meth and it takes alot less.  Swim hasnt even done a half gram and been up for 3 days. 

AND YOU CAN EAT!!!!!!!!!!!!!!!!!your not hungery, but unlike meth, you can eat a cheeseburger!!!!!great, great, sythn. 

Also sex is Great!  My girlfriend.......well anyway

SWIM DID ALSO wash the white crystals by dissolving them in ISO. 70% and letting evaporate. Nice clear pecies that burn clean.

Dont use TOO MUCH sodium bicarbonate in the last step cause it will come out in your 4mar.  If this happens just dissolve as much as you can in Room Temp. ISOPRO. then filter the iso from the white shit that wont dissolve. Evaporate iso and there you go......

[Rhodium]

Now the only thing we need is a working procedure for producing the hydrochloride salt of 4-MAR... HCl in IPA added to an etheral solution of the freebase does not produce a crystalline product.

[Bandil]

yeah, that's definately true. Swim tried to crash some salt crystals by titrating an IPA soln. of 4-mar and adding acetone without a fleck of a crystal. Quite disapointing actually. Drew of the solvent with some vacuum and heat, which produced goo.

I think that the old fester journal suggests gassing in benzene. Does anyone know if that actually works?

But other than that, would the only reason for making the hydrochloride be to enable the user to snort it without to much pain?

Regards
Bandil

[Rhodium]

That is one reason, other reasons include better storage stability, and probably even higher purity upon recrystallization of the salt (even though the substance is ~95%+ pure on ¹H-NMR after recrystallization of the freebase).

[moedank]

Even beeing a person that has a hard time sniffin anything, the bite wasnt that bad.  Rather snort this than cut coke or mdma. Meth has a worst drip than the 4mar, but i still like meth better.   

[Rhodium]

Even if it doesn't hurt that much to insufflate the freebase (4-MAR being a relatively weak base), the water solubility is low enough for the absorption to not be especially effective.

[Bandil]

We'll i can see that we need the salt somehow. Swim's quite willing to experiment to find a suitable method.

Any bright ideas? How about forming the sulfate in IPA/Acetone perhaps?

The original Eleusis used benzene to form the salt in, which is quite non-polar. Maybe pet. ether could be used to crash the salt?

Regards
Bandil

[Rhodium]

I think that slow gassing of the freebase (dried in a vacuum desiccator) in chilled ether (dried over sodium or molecular sieves) with rigorously dried HCl gas (bubbled through a few cm of H₂SO₄ in a gas washing bottle) will do the trick.

If it still oils out, then chilled toluene should be tested (but not as the first option, it is hard to remove without multiple recrystallizations from low-boiling solvents).

[Dextrose]

SWIM made fine glass-like, indeed snortable crystals, using Acetic Acid...

[Rhodium]

How? From what solvent did you precipitate it, and/or recrystallize it from?

[Dextrose]

Sorry for the lack of details.

SWIM was at a friends house, and had brought a little of the freebase with him... A few hundred miligrams was put in a test-tube, with a little denatured ethanol, and concentrated (32%) AA (the only acid SWIM could find in the house   ) was added, until the freebase dissolved in the alcohol...

It was then poured onto a plate, and evaporated in the oven.

No recrystallization was done, since time was a factor in this particular case... (Crashing would probably had worked, but SWIM wasn't sober   )

[Sandman]

SWIM's Merk 11th Ed. doesn't list any uses for KOCN (Potassium Cyanate, correct?).  Is it used in any common OTC products that anyone knows of?

[moedank]

shit son just do a search on yahoo for info on kocn!

It was used in the FIRST ORGANIC SYNTH. EVER!  The synth. of Urea.  I very common synth for starting chemist and nobody even blinks when you ask about it.