2C-I sulfate problems

iohaie · Wed Aug 03, 2005 6:30 pm

alright fellas, how you all doing? been here for a while, glad to see the sites back up, even tough im a bit paranoid bout it.
anyway...
The Great Iohaie tried to make some 2ci. so he purchased 2,5-dimethoxybenzaldehyde, made it into the nitrostyrene via ethylenediammonium catalyst, and then reduced with Al/Hg. Iohaie got a clear amber oil which is 2ch.
so Iohaie went on and iodinated via Oxone/KI. after it was all done, the product was cleaned via A/B, and then dissolved in Xylene.
now it was time to turn the 2ci into sulfate. so iohaie started dripping slowly 98% CP grade Sulfuric acid. after some time, fine xtals apeared. along with some nasty green layer which was very thick and was not miscible. so Iohaie took it off the stirrer, and set up the Buchner funnel. Iohaie started filtering and as soon as the green layer (which actually settled to the bottom under the xylene) hit the paper filter, it MELTED IT, taking with it the precious 2CI xtals!!!
Now, Iohaie is lost for words. what is this nasty grren layer? Can some1 maybe give us a hint?

icecool · Insistent Chemist

Maybe decomposition of some chemical you used or xylene sulfate or something I don't know if it even exists.
But you should drop 98% H2SO4 on it it destroys things insted of making the sulfate.
You should dissolve the sulfuric acid in isopropylalcohol and make a 30% solution in that.
And then add it to the xylene or better dissolve the 2C-I freebase in IPA and then drip the sulfuric acid 30% solution in IPA in there.

anime · Wed Aug 03, 2005 9:27 pm

why not HCL?

It is easy to make HCl crystas of 2CI. Since 2CI does not dissolve well in water you can dissolve the oil in GAA and drip HCL, the 2CI crystals should fall out.

iohaie · Wed Aug 03, 2005 9:55 pm

Much thanks to both of you guys for anwering so quickly. On the next batch I will try both ways and report back, maybe even with pictures... THANKS A BUNCH!

primathon · modified

A little bee buzzed in my ear (from a direction I didn't expect, actually), and told me this:

iohaie · Thu Aug 04, 2005 1:42 pm

Primathon, good to hear from you.
It seems like this paper discusses methoxyamphetamines. It seems quite nice and an efficient way to iodinate, but im pretty sure KI/Oxone works...
Love to hear any other votes from any other bees round here...
would be wierd if rhodium didnt say anything bout it before in his site.

iohaie · Thu Aug 04, 2005 6:56 pm

Howdy... I found out 2 posts from the ol' arcHive supporting 2ch iodination via KI/Oxone :
Barium : A little 2CI perhaps and Del72 : 2C-I

sounds pretty sound.....[/url]

anime · Thu Aug 04, 2005 10:08 pm

since you are using the Al/Hg method for reduction you can iodinate the dimethoxybenzaldhyde to yield the 4-iodo compound. NIS can be used along with I2+Silver nitrate. The resulting nitrostyrene will not be dehalogenated at the reduction step.

Btw, what are your yields like using Al/Hg for reduction?

Alice · Fri Aug 05, 2005 1:15 am

and wtf is that green goo u talking about????
sounds like the mutagen stuff from ninja-turtles Smile

melt the paper????

iohaie · Fri Aug 05, 2005 7:32 pm

anime, yields on small runs are pretty good sound... from 10g nitrostyrene iohaie got about 80% yield. When 50g of nitrostyrene was tried yields dropped like crazy to 5.7g 2ch (pretty pure).
and alice, iohaie have no idea what this green goo was. but iohaie is no ninja turtle (yet!)

Ephoton · Sat Aug 06, 2005 6:48 am

I think you might have cleaved the iodine off the benzene ring and made a polar
solution of h2so4 and iodine (few organics and shit to help with green)

i would next time put the acid in a solvent to dilute it then add it.

are you 100% sure that your amine was real did you gas your 2ch in np
with hcl to get a pure sample.

you need to keep a full record book otherwise it is very hard to
answer these questions. I understand the need to keep the process
undocumented but to get help it is critical.

iohaie · Sun Aug 07, 2005 4:10 am

Ioahie has a report to make :
Iohaie today looked at the liquid which is xylene, supposedly 2ci sulfate and some wierd green goo with residues of paper (from the melt down). It has been sitting in the fridge undisturbed for 2 weeks almost. and to Iohaie's amazment there are clear white xtals in there. looks like something around 100-500mg of fine white xtals, and 1 big needle like xtal. Iohaie thinks this is 2ci... could this bee?

icecool · Insistent Chemist

SWIM is currently waiting 36 hours for the nitrostyrene to form.
It spontanously formed after 50minutes of stirring and now it is standing for 36 hours at room temperature without stirring.
Then it will be filtrated and washed etc.
SWIM is going to do an Al/Hg reaction on it, could you give some more details on the reduction concerning how much Al vs nitrostyrene and was the nitrostyrene added all at once to the Al or was the Al added in portions(and what would be bad about adding Al in portions anyway?).

iohaie · Wed Aug 10, 2005 2:13 am

icecool, for Iohaie the nitrostyrene is very easy to make. the hard part was to get all the benzaldehyde into the solution.
Iohaie says that he waited 36 hours as well, but for him, it all xtalized after maybe 28 hours and settled to the bottom. at first it was like a hard brick of very orange xtals, kinda looking like those big xtal rocks u can buy at xtal shops. Iohaie then braked the big xtal into small xtals. he did not rextalize.

radio879dmt · Wed Aug 10, 2005 6:46 am

Man, other than to learn, dunno why in a dream you would want to make 2C-I, when its available for 80/gram, or in bulk (50g+) at 30/g.

I'd rather, in a dream, get some 2C-I and then make some 2C-TFM which is much more desirable if accidently eaten, in a dream of course.