Yes I did, I posted about it on the "old" hive using the nickname "Zorohustra", I will post it again below:
"Wow, what a complex dream I had last night!
In this dream I dreamed that I tried Eleusis’s ”Proposed nitro -> amine reduction for general use” (which can be found at Rhodium’s outstanding page, check it out!).
13g of GOOD phenyl-2-nitropropene was dissolved in 150ml Glacial Acetic Acid in a 500ml 3-neck RB.
55g of tech. Zinc powder was ”purified” as in Vogel’s 5:Ed. (washing with 10% HCl, then dH2O, followed by acetone).
The dry and pure Zinc was slowly added to the nitropropene solution, while stirring at 700rpm. When ~2/3 of the
Zinc had been added the solution turned ”rust-red”. When all the Zinc had been added the temperature was 80C.
The solution was still stirred at 700rpm, the goal was to heat it to 100C, but it became 106C, at which point it boiled(?!). The solution was no longer “rust-red”, the Zinc was again gray and the solution appeared to be light-pink/red (observed by stopping the stirring for a while).
The stirrer speed was increased to 1100rpm and the solution was held like this for another 30min (total time ~45min). The solution is now light yellow, with some colorless foam.
”Perhaps I have made P2P instead the chemist thought.” (I think I’ve read in March that it can be made with
Zn/HOAc).
60ml 37% ACS hydrochloric acid is put into the additionfunnel and added over perhaps 20min, no spectacular
reaction at all. 1-2 hour later another 20ml hydrochloric acid is added, can’t hurt I mean.
The solution is now near colorless, its decantated from unreacted Zinc, the solution dumped into 1000ml cool dH2O, the Zinc washed with 100ml dH2O.
The solution was washed with 3*60+50ml DCM (500ml sep. funnel
. Then basified with NaOH solution until pH 10-11, then extracted with 3*70+50ml DCM.
The solvent was removed by destillation, leaving VERY LITTLE of ”something”, 15ml anhydrous acetone was added and 2-3 small drops of 98% sulfuric acid, crystals percipitated. But we are talking about a yield in the 100mg range… The chemist dumped it all out, being more of a curios chemist then a desperate speedhead.
The washings was also stripped from solvent by destillation and then dumped into a satured bisulfitesolution, but no crystals formed.
Hmm, IF this reaction can give an acceptable yield this is at least NOT the way to get it, there is really not much to do then but to try with lower temperature, but I am not motivated."
-Methaco(s)mic
