Brominating 2CH HCl directly worked without a snag

[Rhodium]

https://www.thevespiary.org/rhodium/Rhodium/chemistry/edda.html

[Sunlight]

I tried the Ni2B reduction of the nitrostyrene with NiCl2 and NaBH5 in methanol, and yields were similar, I believe to remember about a 15-20 %, I posted it in the Hive. It is not the way to go, anyway it's good to see we have consistent results.

[SpicyBrown]

Well the NMR is back up and useable, although there are issues with locking and shimming, giving some peaks "shoulders" and occaisionally causing standard singlets to split. Thing needs some work. Anyways, the aforementioned 2c-b was analyzed post-bromination with trituration w/EtOAc as only purification method. Sample was prepared in D2O. Here are the peaks present on the spectra. SWIM has no scanner, but could always take a digicam picture of this if anybody really wanted to see it.    Also the sample was very dilute; the solvent peak is huge compared to the 2c-b peaks, integration is a little wacky.

triplet, ~2.95ppm integration 1 (should be 2)
triplet, ~3.21ppm integration 1.5 (should be 2)
two identical singlets, 3.82ppm and 3.86ppm, overall integration 8.5 (should be 6)
broad peak from ~4.6ppm to ~5ppm centered at 4.80ppm (D2O solvent peak, integration in the 100's)
singlet (sharp) at ~7.02ppm, integration 1 (should be 1)
singlet (sharp) at ~7.32ppm, integration 1 (should be 1)

SWIM thinks this looks fine. There are no other peaks present, not even peaks for EtOAc to SWIM's surprise.

-SpicyBrown

[Rhodium]

With such a dilute sample, you will have a hard time distinguishing any impurities from the baseline noise. Could you take a GC spectrum to find the purity of actual 2C-B freebase?

[Oxygen69]

Wouldn't the procedure produce 2C-B HCl instead of 2C-B HBr?

Oxygen69

[Rhodium]

I have addressed this earlier in the thread.

The chloride and bromide ions can interchange freely creating a mixture of salts of varying solubility (making isolation difficult), so after washing the filtered dark crystal mass on the buchner funnel with a little cold acetic acid (must be done, or you won't get rid of the black impurities), it is highly reccommended to follow up with an acid/base extraction and reprecipitation of the HCl salt as in

Pihkal #20.

(http://www.erowid.org/library/books_online/pihkal/pihkal020.shtml)