反应详情

To a stirred and cooled (0° C.) solution of 48 parts of 4-chloro-N,N-bis(4-fluorophenyl)butanamide in 108 parts of tetrahydrofuran were added 240 parts of a solution of borane, compound with thiobismethane, in tetrahydrofuran. After stirring overnight at room temperature, the reaction mixture was decomposed with 160 parts of methanol. After evaporation, The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and petroleum ether (20:80 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 32.5 parts (91.5%) of N-(4-chlorobutyl)-4-fluoro-N-(4-fluorophenyl)benzeneamine as a residue (int. 70).

1. stirringAfter stirring overnight at room temperature
2. customAfter evaporation
3. customThe residue was purified by column chromatography over silica gel using
4. additiona mixture of trichloromethane and petroleum ether (20:80 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated