Ridiculum - 24-10-2005 at 11:19
In accordance with the formula below swim conducted a couple of experiments.
R'COOH + 2KOH = R' + K2CO3 + H2O
Swim mixed 25g of nicotinic acid with 100g of Sodasorb in a mortar. The mixture turned light purple. This was put into a 500ml flask, attached to the
distillation apparatus, and heated with a propane torch. The mixture turned dark purple and then upon further heating and application of a light
vacuum, water started coming over. Around 10-15 ml, that had a faint smell of pyridine. At this point, the purple color was completely gone. Snow
white powder was left in the flask... and upon further heating no pyridine distilled over.
In a related experiment:
Swim mixed 25g of nicotinic acid with 36g of KOH (roughly 1:2 molar), and a 1/2 a cup of water in a 500 ml distillation flask, attached it to the
distillation apparatus, and started heating the flask with the propane torch. As most the water evaporated, the remaining snow white gue started to
solidify on the flask. At this point swim switched the receiving flask on the distillation apparatus. Now light vacuum was applied (10-15-20 mm Hg
using a hand pump). The parts of the powder that were exposed to the heat for a prolonged period started to change color, first to green, then to
brown. As it turned to brown it boiled and pyridine started to distill over...
A substantial amount of pyridine /water distillate came over (25-30ml). It had a pungent odor of a concentrated pyridine solution. Swim did not finish
clean up yet, so pyridine yield is undetermined. But it is good enough for swim to try it again on larger scale....
The flask that this procedure was done in is completely destroyed...Warped in placed by the torch, completely stuck full of black brown never will get
it off crap...cracked upon cooling...so on...
Any ideas on improving this procedure, apparatus would be most appreciated.
IPN - 24-10-2005 at 11:41
You might wan't to read through the benzene synthesis thread . Using a wine bottle or a tin can with a copper condenser will be much cheaper and better option for a decarboxylation apparatus.
tumadre - 24-10-2005 at 11:51
nicotinic acid can be confused with niacin and niacinamide, nicinamide is what they have in otc vitamin supplements, I have a bottle that, among other
things contains approximatly 300 grams of nicinamide. this would certainly be cost effertive, but I do not believe nicinamide will work with this
chemistry.
is nicotinic acid cost effective? how much does 25 grams cost?