反应详情

Di-tert-butyl carbonate (996 mg) was added to a mixture of 2-benzhydrylpiperazine dihydrochloride (1.65 g) and N,N-diisopropylethylamine (3.5 ml) in N,N-dimethylformamide (17 ml) under ice-cooling. After being stirred at same temperature for 2 hours, the mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with brine, dried over sodium sulfate and evaporated under reduced pressure to give a crude oil. The oil was purified by column chromatography on silica gel using a mixed solvent of dichloromethane and methanol (50:1) to give 1-tert-butoxycarbonyl-3-benzhydrylpiperazine (1.26 g) as a colorless powder.

1. temperaturecooling
2. extractionextracted with ethyl acetate
3. washThe extract was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customto give a crude oil
7. customThe oil was purified by column chromatography on silica gel using a mixed solvent of dichloromethane and methanol (50:1)