反应详情

温度

80 °C

1-(2-Chloro-4,6-dimethylphenyl)piperidin-2-one (18.8 g) and Lawesson's reagent [2,4-bis (4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide] (19.2 g) were combined in 150 mL toluene and the mixture was stirred in an 80° C. oil bath for 3 h. The reaction mixture was then cooled to room temperature and filtered. The filtrate was concentrated on the rotary evaporator and the residue was chromatographed on silica gel, eluting with 9:1 hexane/acetone, to provide 19.4 g of 1-(2-chloro-4,6-dimethylphenyl)piperidine-2-thione: mp 146.8-148.0° C.

1. temperatureThe reaction mixture was then cooled to room temperature
2. filtrationfiltered
3. concentrationThe filtrate was concentrated on the rotary evaporator
4. customthe residue was chromatographed on silica gel
5. washeluting with 9:1 hexane/acetone