反应详情

To a stirred solution of 17 parts of (4-fluorophenyl) [1-(1-methylethyl)-1H-benzotriazol-5-yl]methanone in 80 parts of ethanol were added 3.4 parts of sodium tetrahydroborate. After stirring for 1 hour at room temperature, the reaction mixture was neutralized to pH 7. The reaction mixture was concentrated and the product was extracted with ethyl acetate. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of dichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 10.7 parts (62.5%) of α-(4-fluorophenyl)-1-(1-methylethyl)-1H-benzotriazole-5-methanol as a residue (int. 4).

1. concentrationThe reaction mixture was concentrated
2. extractionthe product was extracted with ethyl acetate
3. customThe extract was dried
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography over silica gel using
7. additiona mixture of dichloromethane and methanol (98:2 by volume) as eluent
8. customThe pure fractions were collected
9. customthe eluent was evaporated