11-13-03 07:01
No 470603
This is a work of fiction:
A researcher recently made his fifth attempt at synthesizing 2C-B HCl. He weighed 14.67 g of 2C-H HCl, dissolved it in H2O, basified with 25% NaOH, and extracted with 4x10 mL DCM. The solvent was stripped, the freebase was mixed with GAA, and bromine in GAA was added. The reaction mixture turned black
and was allowed to react for several minutes as the researcher ate dinner. After the researcher had returned, he noted that the mixture had taken on a look somewhat resembling toasted marshmallows. The mixture was filtered, and the filter cake was washed with GAA (making it almost white) and dissolved in H2O. The solution was basified with 25% NaOH and extracted with 4x10 mL DCM. The solvent was stripped, and the dark brown oil was distilled at 111 C under extremely high vacuum with no condensor, leaving a clear oil that froze in an ice bath. The oil was dissolved in H2O with GAA and 2C-B.HCl was precipitated by the addition of 37% HCl. The mixture was filtered, and the filter cake was washed with H2O and DCM. DCM is a very poor substitute for ether for this (it appears to dissolve 2C-B.HCl slightly), but ether was not available. After drying and grinding, the white powder weighed 10.17 g (51%).
Woohoo!
(Hive Bee)
11-13-03 07:14
No 470606
I think you mean 2C-B.HCl, not 2C-H.HCl. Otherwise OK.
"The oil was dissolved in H2O with GAA and 2C-H HCl was precipitated"
(you can always take some more)
11-13-03 09:18
No 470615
The solvent was stripped, and the dark brown oil was distilled at 111 C under extremely high vacuum with no condensor
I have heard that this is illegal in quite a number of countries, and punishable by whipping! How on earth did you avoid part of the 2CB freebase entering your pump? I suppose you have distilled directly into a RBF? Not all of the gas will hit the sides of the walls and condense. At that stage i wouldn't dare doing such a thing without condensing!
Regards
Bandil
I just love the smell of bromine in the morning!
(Chief Bee)
11-13-03 16:28
No 470661
How on earth did you avoid part of the 2CB freebase entering your pump?
He didn't, he only got 50% yield, the rest was sucked into his pump, safely stored there as evidence.
(Stranger)
11-13-03 19:53
No 470680
His oil weighed about 10.5 grams after distillation. If he tries this again, he will use ether.
(Hive Bee)
11-14-03 22:19
No 470916
Swim has obtained a quantity of 2,5-DMPEA HCl salt.. can one just dissolve this HCl salt in GAA and add bromine dissolved in gaa or is it necessary to basify/extract? Would toluene be an effective solvent for extraction of the 2c-h freebase?
(Chief Bee)
11-15-03 02:37
No 470959
You need to basify/extract, or you'll end up with a mixture of hydrobromide and hydrochloride salts afterwards, adding a lot of problems to your workup/purification.
Toluene works, but DCM or chloroform is preferable.