"I have done this rxn using 48% aq HBr and HCl(g) and produced 70% returns of perfect bromosaf MANY times, it does work."
Ritter
Is this the procedure you used?(shown Below)
And would you care to comment on any optimizations?
Such as temp, I would assume colder is better?
HCl(gas) addition rate?
Thanks
Foxy
PREPARATION OF BROMOSAFROLE FROM 48% HYDROBROMIC ACID
A greatly improved procedure using 48% HBr to make bromosafrole is my own
invention, and it is with unbounded pride that I offer this advance to the
field of MDA manufacture. This procedure is both quicker and much higher
yielding than the procedure worked out by the jackass who wrote the article
for the Alabama Academy of Science cited earlier. This so-called researcher
was hired by the DEA to fool around with 48% HBr to see if it could be used
to make MDA or MDMA from sassafras oil. They had busted someone with 48% HBr
and a load of sassafras, and to make their case they needed to show that it
could be done. The result is a testimonial to the power of money - for it,
some people will say anything. I just wonder who is rotting away in a cage
as a result of his inflated claims.
You bought this book for the straight poop, so let your Uncle be your guide.
To get good yields of bromosafrole from 48% HBr and sassafras oil, mix one
part sassafras oil with one part glacial acetic acid and two parts 48% HBr
in a suitable-sized flask. Chill this mixture down in ice, then with strong
magnetic stirring pass a stream of dry HCl gas into the solution for about
an hour. See Chapter 5 for the dry-HCI gas-generator. How much HCl to pass
into solution? Well, for a batch using 50 ml of sassafras oil, the amount of
dry HCl generated by dripping 75 to 100 ml of sulfuric acid onto a half-full
500 ml flask of salt-hydrochloric-acid paste is about right. A little bit
more wouldn't hurt. Good ventilation is required!
As the dry HCI passes into the solution, it dehydrates the 48% HBr, causing
it to react with the safrole. The dehydration and the reaction both generate
a good deal of heat, so fresh ice will periodically have to be put into the
bath around the reaction flask. The temperature of the reaction shouldn't
be allowed to rise above 10-15° C. The reaction mixture first turns green
then blue, then purple, and finally burgundy. When the bubbling with dry
HCl is finished, stopper the flask and continue stirring in the cold for two
days. Sometime around a day into this stirring, no separation of phases can
be seen when stirring ceases.
https://www.thevespiary.org/rhodium/Rhodium/chemistry/halosafrole.txt
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