OK Foxy, I got off my fat arse and went to the libary and did some more searching i found that:
The dry powder thingy was infact
ethylenediaminetetraacetic sodium salt (cas 64-02-8)
& sodium sesquicarbonate (cas 533-96-0)
basically not what one is lookin for huh!
cause EDTA is not EDA, which from lookin around EDA is what
everyone wants for the birch reaction.
But I did find this on re-reading old posts......
04-21-00 No 108534
Preparation of 3,4-methylenedioxyphenyl-2-nitropropene (from piperonal)
In Pihkal, Alexander Shulgin mentions that the preparation of
MDP-nitropropene can be carried out in cold methanol with aqueous sodium
hydroxide as the base. In fact, this method is even more reliable, and
gives higher yields than the other method advocated by the dear doctor in
his book.
15g of piperonal was dissolved in 40ml of methanol under stirring in a
250ml Erlenmeyer flask. When all of the piperonal had dissolved, 7.1g
nitroethane was added to the solution. The flask was put in a ice/salt-bath
with magnetic stirring, and when the temperature of the solution had
dropped to 0°C, an ice-cold solution of 4g of NaOH in 20ml dH2O was added
at such a rate that temperature never rose above 10°C. A white precipitate
formed at the bottom of the flask during this addition, which was broken up
with a glass rod. The stirring was continued for another hour, while the
temperature of the solution was never allowed to rise above 5°C, and at the
end of this time, 100 ml of ice-cold dH2O was added to the solution, which
caused even more precipitation of white solid. The whole slurry was poured
into 100 ml of ice-cold 2M HCl solution in a 500ml Erlenmeyer flask, which
was gently swirled, and there was a slight bubbling and fizzing, with the
color of the solution shifting from white to blue to green to yellow in
under a minute. Quite spectacular! When the fizzing had subsided, the
solution was once again placed in in an ice-bath with magnetic stirring.
When the temperature had dropped to about 5°C, the solution was clear with
yellow granules of crude product at the bottom. The granules were filtered
with suction, and recrystallized from IPA. After air-drying, the
canary-yellow crystals amounted to a yield of 65-70% of theory.
So if I read the post correctly Naoh is used as base instead of any of the amines?
?
I do not have TS2 but every other bee that does already new this I guess.
Back to the drawing board for making nitroethane without all that DCM.........still waiting for your follow up post Obit!!
cheers Foxy2
