反应详情

温度

80 °C

To a room temperature solution of ethyl 4-[(4-fluorophenyl)thio]-3-oxocyclohexanecarboxylate (3.4 g, 11.5 mmol) in dichloroethane (100 mL) was added AlCl3 (3.7 g, 27.6 mmol). The mixture was heated to 80° C. for 1 hour. After cooling to room temperature, the reaction was diluted with water and acidified with 1 N HCl. The aqueous mixture was extracted with EtOAc. The organic layer was washed with water then brine, then was dried over MgSO4 and concentrated to an oil. Purification by chromatography on silica gel afforded 2.5 g (77%) of the title compound as semi-solid: MS (+) 278 (M)+.

1. temperatureAfter cooling to room temperature
2. extractionThe aqueous mixture was extracted with EtOAc
3. washThe organic layer was washed with water
4. dry with materialbrine, then was dried over MgSO4
5. concentrationconcentrated to an oil
6. customPurification by chromatography on silica gel