反应详情

A mixture of N′-benzylidene-4-trifluoromethylbenzohydrazide (2.92 g), thionyl chloride (1.09 ml) and toluene (50 ml) was heated under reflux for 1 hr. After cooling, the reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, volume ratio) and recrystallized from hexane to give N-benzylidene-4-trifluoromethylbenzenecarbohydrazonoyl chloride (1.85 g, yield 59%) as pale-yellow plate crystals. melting point: 95–96° C.

1. temperaturewas heated
2. temperatureunder reflux for 1 hr
3. temperatureAfter cooling
4. concentrationthe reaction mixture was concentrated
5. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, volume ratio)
6. customrecrystallized from hexane