反应详情

Aminoguanidine hydrogen carbonate (1.24 g, 9.1 mmol) was added to a solution of concentrated hydrochloric acid (0.8 cm3, 9.3 mmol) in water (3 cm3). After diluting the resulting solution with ethanol (20 cm3), 2,6-dichloro-3-nitrobenzaldehyde (2.0 g, 9.1 mmol) was added and the mixture heated under reflux for 7 h. The solution was evaporated under reduced pressure and the residual solid suspended in refluxing ethanol, basified (pH 11) by addition of dilute sodium hydroxide solution and cooled to yield a white solid which was collected. This solid was dissolved in hot methanol and the solution acidified (pH 2) with ethanolic hydrogen chloride, diluted with diethyl ether and cooled to yield (2,6-dichloro-3-nitrobenzylideneamino)-guanidine hydrochloride as a white solid, m.p. 186°-7° C.

1. additionwas added
2. temperaturethe mixture heated
3. temperatureunder reflux for 7 h
4. customThe solution was evaporated under reduced pressure
5. temperaturein refluxing ethanol
6. additionby addition of dilute sodium hydroxide solution
7. temperaturecooled
8. customto yield a white solid which
9. customwas collected
10. dissolutionThis solid was dissolved in hot methanol
11. additiondiluted with diethyl ether
12. temperaturecooled