反应详情

Dissolve 568 mg (2.2 mmole) of 2-fluoro-7-hydroxymethyldibenzo[b,f]thiepin in 30 ml of methylene chloride and add 647 mg of 98% pyridinium chlorochromate. Stir the mixture and follow the reaction by thin layer chromatography (Merck silica gel F254 with 5% ethyl acetate in toluene). When complete, filter the mixture through a bed of Florisil, and wash through with methylene chloride. Evaporate the filtrate to obtain a brown solid (600 mg). Purify the crude product by chromatography on silica gel using totluene as solvent to obtain the title compound as a yellow solid, m.p. 137°-139° C.

1. filtrationWhen complete, filter the mixture through a bed of Florisil
2. washwash through with methylene chloride
3. customEvaporate the filtrate