2CB.HCl synthese

icecool · Insistent Chemist

There wasn´t a topic about this already.
So I made one.
And I want to ask some questions concerning the syntheses.
If I would make 2CB.HCl, I would go about making the nitrostyrene of 2,5/diMeOBzCHO in nitromethane and EDDA.
Then with the nitrostyrene, I would do an Al/Hg reduction, and THEN.
Do and a/b purification, after doing that you would have an oil in ether right (after you extracted it).
And if you would gas that anhydrous ether which includes the 2C-H then you would get 2C-H.HCl is that crystaline?
And then I would make a solution of 2C-H.HCl in glacial acetic acid.
Then dropwise add to that the correct molair amount of bromine which is made in situ by adding H2O2 and DCM and NaBr and H2SO4 37% together in a dropping funnel, and adding that to the 2C-H.Ac in HAc. The NaBr would be in solution and after adding H2O2 dropwise to the dropping funnel Br(g) would evolve which will dissolve in the DCM after that the dropping funnel is shaken the Br would go into the DCM and settle down on the bottom so you can drain it into the mixture of glacial acetic acid and 2C-H.Ac
Now there will go a bit water into the DCM since on top of it there is a solution of NaBr.
So the salt that will form 2C-B.Ac will dissolve in the little amount of water present won't it?
Then one would have 2CB.Ac right?
One would like to make the 2CB.HCl so I read that it the hydrochloride is insoluable in water, WHY?
I thought all the hydrochlorides were hygroscopic and very soluable in water.
But okay then this one isn't, so if one would bubble HCl gas threw the 2CB.Ac solution in glacial acetic acid there would 2CB.HCl preticipate?
Couldn't one just add 37% HCl to it then too insted of bubling it?
and one could also add a pre made DCM+HCl solution when one would bubble HCl gas threw DCM so it would dissolve in that then you can measure out the exact amount what you need.
So I guess HCl gas dissolves in DCM?

anime · Thu Jun 23, 2005 12:32 am

I personally would avoid gassing the ether solution and instead perform a distillation on the amine to get something nice and pure. Dissolve the amine in GAA and proceed with the bromination. There is no need to gas unless you absolutely have to.

transistor child · gnome

And gassing 2C-B in GAA is a bad idea. You need to do a A/B extraction and gas the organic layer (toluene or something similiar). I would advise you to read up on some basic organic chemistry and laboratory safety before atempting any synthesis. It's fun, and you'll learn a lot.

icecool · Insistent Chemist

I've already done quite some synthesis :S
I just had some questions about this one.
I know how to purify and I won't distill since it is a too great loss.
So I will do an a/b purification.
But why do some people dissolve the freebase in GAA and why do some people dissolve 2C-H.HCl dissolve in GAA.
That was the question.
And then adding DCM+Br(g) to it to brominate it.
But then the next question after brominating it.
You will have 2C-B.Ac
It could then also be turned into the HCl salt by adding HCl 37% since the hydrochloride is insoluable in water.

icecool · Insistent Chemist

I've already done quite some synthesis :S
I just had some questions about this one.
I know how to purify and I won't distill since it is a too great loss.
So I will do an a/b purification.
But why do some people dissolve the freebase in GAA and why do some people dissolve 2C-H.HCl dissolve in GAA.
That was the question.
And then adding DCM+Br(g) to it to brominate it.
But then the next question after brominating it.
You will have 2C-B.Ac
It could then also be turned into the HCl salt by adding HCl 37% since the hydrochloride is insoluable in water.

braindamage · Wed Jun 29, 2005 9:01 pm

goddamn i havent visited this site for a while..
IMO using 2ch.hcl wont work well or maybe at all,you have to use the freebase,so first use ~40% water sol of NaOH and 2ch.hcl,extr w nonpolar and than Br it...it worked for swim,but he got 2cb.hbr so than he had to convert it to 2cb.hcl...yeah you guessed it yield loss

the alchemist · Thu Jun 30, 2005 12:05 am

The 2C-B you isolate after addition of Br2 is an HBr salt (which works just fine after a recryatallization). It would be wise to clean up your 2C-H via distillation before bromination to ensure minimal contaminants in your final product. Garbage in = garbage out. Br2 is dissolved in DCM? The synth from PIHKAL uses Br2 dissolved in GAA, am I correct?

icecool · Insistent Chemist

Yeah that is right.
But as you look at the topic about bromine.
You can see that it is a great advantage, to produce Br(g) in situ so with DCM and H2O2 and an acid.
So from an bromine salt (NaBr) the HBr is formed because of the acid then you add an oxidizer which releases the bromine gas, and the bromine gas then dissolves in DCM.
So you don't need to handle this irritating gas, just drip in the DCM and it reacts too.
Anyway now I understand it better with the explanation braindamage thanks a lot.
And can't you use 2CB.HBr insted of 2CB.HCl since then you wouldn't have that loss in yield, or is the HBr salt way more soluable as the HCl salt since the HCl salt is insoluable in water(why is that though normally HCl salts are hygroscopic).
And you will get the 2CH-freebase anyway so you don't need to treat it with NaOH to get the freebase unless you were so stupid to already make the HCl salt.
And what about doing an a/b purification on the freebase insted of distilling it that is where real losses are going to happen.
Unless you have a NS 14,5 distillation setup (well I don't ).
And braindamage how did you turn the HBr salt into HCl salt, as it is not soluable in water you shouldn't need to gass it and another oppurtinity insted of gassing is dissolving HCl gas in DCM so you can calculate the exact amount of HCl added to your PA, and as it is not soluable as I sayd before you could also just add 37% HCl solution right?

braindamage · Sun Jul 03, 2005 8:01 pm

yup swim agrees with the alchemist,if youre making yout own 2ch or freebasing it from a 2ch.hcl it would be wise to distill it before the bromination step.mind you swim didn’t do this but that’s because he at that time thought he was smarter than the rest of the world.now he just thinks hes smarter than the population of Botswana,and maybe Trinidad and Tobago …..ranting,sorry

As for elemental Br,well swim preferred it.why-because hes a weird fuck,and likes to breathe fumes...no really if you keep it cool enough youll have no problems.Also it would be wise to make a heat sink(i.e. to have a bucket of cold water) if youre using more than 100g of 2ch since the rxn is very exothermic.

the reason why swim made hcl salt is because 2cb.hbr seems to have many forms,especially its hydrates so it may be hard to determine its effective dose,and from the same batch you may need different quantities for the same effect.On the other hand it is water soluble so you can snort it.
One more reason why swim decided to use hcl form is because he wasnt sure what was the final product-which form of 2cb.hbr and what % of 2cb.ac,so he couldnt be sure of the dosing.
why is 2cb.hcl insoluble,well as always it must be a question of the polarity,I guess you can calculate it.

Swim also made a sloppy freebasing of 2cb and the hcl titration,and he still had a pretty good yield,so basically you base the hbr salt with 20-40% NaOH solution,extr w DCM,but you can also use MeCl and some use ether.You can titrate the freebase easily just calculate your ratios-swim used 2cb:hcl=1:1.5(and that’s was in swims opinion too much,),used a 15% Hcl water solution,but you can also use 36%,the more water you have the more it is likely you will get hydrates(which will affect the dosing),the less water you have the more likely it is you will over titrate it… but this synth allows a lot of sloppiness and mistakes,and swim is sure you wont have any problems

Also swim washed the hbr salt w the solution of acetic acid and once w cold ether.the hcl salt was washed w cold dH2O and cold ether great number of times,to boost the pH since he overtitrated it..
He didn’t recryst the salts,because he was a sloppy pig,but you can do so with ethyl acetate or ether(guys flame me please if im wrong)

hope this ranting helps,good luck

daeron

icecool · Insistent Chemist

Thanks a big time for the answers this sure did help a lot!

anime · Sun Jul 10, 2005 10:09 pm

icecool · Insistent Chemist

Won't the crystals just redissolve like with amphetamine sulfate?
So when you save a bit of FB at the beginning you can add some FB again after everything dissolves.
Or just calculate how much you would need when weighing the FB.
But I'll keep the pH in mind and use pH paper.
Will do that too next time when SWIM will make amphetamine.
It is in the wrong topic but at what pH should one stop when making amphetamine sulfate with sulfuric acid adding to the FB at pH 7?

icecool · Insistent Chemist

SWIM made 2,5-dimethoxynitrostyrene with EDDA and it all went fine.
Got 6,03g of the nitrostyrene out of 5g 2,5-dimethoxybenzaldehyde.
And reduced it via Al/Hg he used 10g of Al foil which was shredded in the mixer to little nuggets.
Anyway added MeOH to cover the Al and added 80mg HgCl2 in two portions.
When amalgamation started the nitrostyrene was added all at once which was dissolved in 50ml GAA and 30ml MeOH.
The reaction was carried out in a 1 liter RBF, first 4g of Al was in the RBF and later on when almost everything dissolved more Al was added to keep the temperature around 60*C.
Extracted 2 times with 100ml and again 100ml toluene.
Dried over MgSO4 and rotavapped off the toluene, then an acid base purification was done.
With H2SO4 and washed with DCM (3x) then added NaOH 20% until white cloudiness persistet, and toluene was added and more NaOH was added. toluene dried again and rotavapped.
Got around 5ml of 2C-H (still contained a bit of toluene since it was only rotavapped and not distilled in a "real" distillation setup.
light yellow and turned brown because of the CO2 in the air.
Then dissolved it in 12ml of GAA nothing happened here, no exothermic reaction or white crystals or something like that (it was in an ice/salt bath though! the 2C-H had been standing in there for like 15minutes) then the GAA was added to it).
So it could not have heated up because of the ice/salt bath, and it was stirred while adding GAA by magnetic stirring.
Then Br was added by the method descriped before here which worked very well.
It was done this way, 8ml DCM, 30ml H2O 2,4g KBr and 16ml 30% H2SO4 and 0,97ml 30% H2O2.
It was shaken well and the DCM layer got dark red this was added to the mixture of GAA and 2C-H the mixture heated up a little bit from 5*C to 20*C.
No fumes what so ever, then the mixture was just red...no brown paste or crystals.
And after 12 hours it was heated to the BP of DCM (43°C) for 10minutes and then put in the freezer at -18*C
Nothing froze when checking later (5 hours), only very few white crystals, don't even know if it are actually crystals or something else...
What could have happened what did SWIM do wrong, did SWIM use too much Br or did SWIM do something wrong with the Al/Hg reaction?
Could it maybe be that there was still a bit of toluene mixed with the 2C-H so the 2C-H didn't get brominated but the toluene did or the toluene interupted the bromination?
Or is the reaction just milder because it was done with DCM, so the Br was added in portions since it needed to be extracted like 5 times.

Thanks in advance Ice

EDIT: Made me think reading the report on the synthese of Dr. Gonzo, he sayd 2C-B.HBr is "much-soluable-expected." I guess he means that it dissolves quite well in acetone.
Since I used quite some DCM like 15-20ml or so couldn't it very well be that it dissolved in the DCM?
If there aren't more crystals later on the day then I'll evaporate the DCM and leave the 2C-H (plus a bit of toluene) and the pure bromine and around 12ml of GAA together and see if it forms crystals then or reacts then....

anime · Mon Aug 15, 2005 9:44 pm

I'd do this. make the solution basic. Add a little more dcm (50-100ml). Extract. Get the resulting crude oil, dissolve in IPA and drip HCl onto that IPA.

icecool · Insistent Chemist

So no filtration first?
Just basyfing the whole crap mixture of everything.
Including bromine and everything?
Well I already filtered it since I came to the conclusion it couldn't hurt...
Just to see what would stick in there.
I wetted the filter with ice-cold ether.
And then poured the mixture over it.
Sucked it air-dry with vacuum filtration.
and now the filter is light brown I guess it are crystals only a VERY little bit but that doesn't matter as long as it works for the first time Very Happy

Anyway SWIM just let's it dry further in the air since it is washed with ether 2 times quickly.
So it should be gone quickly.
Then scrap everything off the filter as much as possible.
And then convert it to the hydrochloride (if SWIM still wants it too then, since that means another loss in yield a very little bit, since it already is only like 20mg in total or so???)