The latest notes from my crazy aunt's diary:
Into a test tube there were placed:
a) 1g of 2,5-diMeO-BA
b) 0,5mls MeNO2 (distilled, but not quite dried - half of it distilled over at ~90 C - MeNO2's azeotrope w/water, 76% MeNO2)
c) 3,5mls MeOH
And the solution was placed into an ice/salt bath at -7 C, where it shortly turned into a fine suspension.
In the same bath 0,9mls of 40% NaOH soln in a small syringe were pre-chilled.
Also one should prepare bee4hand the following things:
a) A 2-5cm3 syringe fitted w/a pipette long enough to extend to the testtube's bottom; chilled in a freezer.
b) Ice-water and a freezer-chilled 10cm3 syringe (chill syringes' parts separately!)
c) A soln of 7mls HCl in 13mls water, kept at RT.
When the temp of the mixtr in the bath falls to -5 C, alkali was gradually added in 3 portions, with vigorous hand-stirring w/thermometer - the 1st time the temp jumps up by ~10 C - make sure that temp falls back to -5C each time.
The mixtr beecame homogenous. It was left in another icebath - temp rising from 6 to 10 C - for an hour.
Then it was chilled back to -5 C and 10mls of ice water is added thru syringe - all turns cloudy-white. As fast as possible, it was
dripped thru the pipetted syringe into the acid soln with vigorous stirring.
Contrary to the documented on Rh's site similar prep'n of MDP2NP, no 'spectacular color shift' was observed - yellow color appeared immediately, and by the end of the add'n the mixtr represents a slurry of bright-orange nitrostyrene xtals of very fine consistency. They are filtered, washed w/water 3 times and air-dried on a saucer to give 0,7g (56%) of product, which has indeed a SPECTACULAR color - each time SWiHKAL looked at it his heart smiled, so cheerful and bright it was
Maybee, somebee will have SOMETHING to say about this?
Any ideas on why the yield was so crappy? Well, still acceptable for a hallucinatory kitchen chemist, i guess.
Yours truly,
Antoncho