反应详情

N-(2-aminophenyl)-3,5-di-t-butyl-4-hydroxybenzamide (0.85 g) and diisopropylamine (0.39 ml) were suspended in dichloromethane (20 ml) and a solution of phenyl chloroformate (16.8 g) in dichloromethane (30 ml) was added dropwise under ice-cooling. After stirring the mixture overnight, the reaction solution was washed with water, saturated saline, dried over anhydrous MgSO4 and the solvent was distilled off. Purification of the residue by a silica gel column chromatography (chloroform:ethyl acetate=10:1) followed by crystallization from hexane/ethyl acetate afforded phenyl N-[2-(3,5-di-t-butyl-4-hydroxybenzoylamino)phenyl]carbamate (12.6 g, 49%).

1. temperaturecooling
2. washthe reaction solution was washed with water, saturated saline
3. dry with materialdried over anhydrous MgSO4
4. distillationthe solvent was distilled off
5. customPurification of the residue by a silica gel column chromatography (chloroform:ethyl acetate=10:1)
6. customfollowed by crystallization from hexane/ethyl acetate