反应详情

温度

0 °C

To a solution of dibenzo[b,f]thiepin-3-carboxylic acid (U.S. Pat. No. 4,536,507 (1985)) (415 mg, 1.63 mmole) in THF (20 mL) at 0° C. there was added methyl lithium in ether 1.4M (2.56 mL, 3.59 mmol); the mixture was stirred at 0° C. for 1 hour, then poured onto a well-stirred saturated aqueous ammonium chloride solution (100 mL). The organic phase was collected, washed twice with brine, dried and evaporated. Column chromatography on silica gel, eluting with a 1:2 mixture of ethyl acetate-hexane, afforded the title compound as a yellow solid (320 mg), m.p.: 82°-84° C.

1. customThe organic phase was collected
2. washwashed twice with brine
3. customdried
4. customevaporated
5. washColumn chromatography on silica gel, eluting with a 1:2 mixture of ethyl acetate-hexane