反应详情

To a stirred and cooled (0° C.) suspension of 23.4 parts of lithium tetrahydroaluminate in 270 parts of dry tetrahydrofuran were added portionwise 45 parts of 1-butyl-1H-benzotriazole-5-carboxylic acid. Upon complete addition, stirring was continued for 1 hour at 0° C. The reaction mixture was hydrolysed with 50 parts of water. The whole was filtered and washed with a mixture of dichloromethane and methanol (90:10 by volume). The filtrate was evaporated to dry and 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 18 parts (42.7%) of 1-butyl-1H-benzotriazole-5-methanol as an oily residue (int. 10).

1. temperaturecooled
2. additionUpon complete addition
3. stirringstirring
4. filtrationThe whole was filtered
5. washwashed with a mixture of dichloromethane and methanol (90:10 by volume)
6. customThe filtrate was evaporated
7. customto dry
8. customthe residue was purified by column chromatography over silica gel using
9. additiona mixture of dichloromethane and methanol (98:2 by volume) as eluent
10. customThe pure fractions were collected
11. customthe eluent was evaporated