反应详情

An ethanol solution (50 ml) of 4-chloro-4'-methylmercaptomethylbenzophenone (9.3 g), hydrazine hydrate (6 ml) and acetic acid (3 ml) was heated for 20 hours with refluxing. The solvent was distilled off under reduced pressure, and then the obtained oily substance was diluted with dichloromethane and washed successively with an aqueous 5% sodium hydroxide solution, water and an aqueous saturated a sodium chloride solution, followed by drying over anhydrous magnesium sulfate. The solvent was then distilled off to obtain 4-chloro-4'-methylmercaptomethylbenzophenone hydrazone (7.1 g) as an isomer mixture (syn form/anti form=about 1:1).

1. temperaturewith refluxing
2. distillationThe solvent was distilled off under reduced pressure
3. additionthe obtained oily substance was diluted with dichloromethane
4. washwashed successively with an aqueous 5% sodium hydroxide solution, water
5. dry with materialby drying over anhydrous magnesium sulfate
6. distillationThe solvent was then distilled off