反应详情

A mixture of 3.6 parts of 4-chlorophenylhydrazine and 2.0 parts of triethylamine in 20.0 parts of toluene was stirred at room temperature for fifteen minutes. To the mixture was added 2.5 parts of 2-cyanocyclohexanone, prepared from commercial 2-chlorocyclohexanone and potassium cyanide [von R. E. Meyer, Helv. Chim. Acta., 16, 1291 (1933)], and a few drops of acetic acid. After refluxing for two hours, followed by stirring at room temperature overnight, the reaction mixture was evaporated to remove toluene and was treated with water, extracted with diethyl ether, dried over anhydrous magnesium sulfate and concentrated. Recrystallization from ethanol/water gave 2.6 parts of the compound, m.p. 140°-142°.

1. temperatureAfter refluxing for two hours
2. stirringby stirring at room temperature overnight
3. customthe reaction mixture was evaporated
4. customto remove toluene
5. additionwas treated with water
6. extractionextracted with diethyl ether
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated
9. customRecrystallization from ethanol/water
10. customgave 2.6 parts of the compound, m.p. 140°-142°