Let me start by sayin wow. To this date this is the easiest synth i ever seen in my life, side from making Hg2I2. From start to finish it takes about 4.5hrs. And it requires no lab glass at all.
Procedure
16.6 gms(.1mol) 2,5 dimethoxybenzaldehyde was finely powered and dissolved in 40mls 99.9%MeOH at RT. It took 30 mins stirring with a spatchula to get it all into solution.
Then 7.1 gms 99% Nitroethane was added.
4gms of NaOH is dissolved into 20ml of H2O and placed into the icebath to cool.
The rxn vessel (Jar) was placed into an ice bath until the 2,5dimethoxybenzaldehyde began to crash out.
As soon as it began to crash out it was removed from the ice.
The NaOH solution was added with a syringe over the period of 10 mins. When all the NaOh was added the whole thing spontaniously crystalized to an yellow white color. It did not heat up at all but still it was placed into the ice bath and stirred by hand for an hour.
100mls of cold H2O was added which did not change much at all.
1l of 2M Hcl was made.(200mlof 36%Hcl in 800mlH2O)
100 ml of the 2M Hcl solution was added into the solution. when each drop hit it made a blue color that turned lime green after a few seconds. When it all was added it bubbled for a few minutes and then was placed into the ice bath. At this point it was canary yellow. the soution was yellow as were the crystals setting at the bottom. I suspect there was more still in solution at this point. the whole thing was put into a filter.
The filtercake was washed 3x with 50 ml of H2O
The crystals were air dried without rxtylization to a weight of 16.2 gms.
I say again wow. Now it is time to try with Nitromethane
VL_