反应详情

To a solution of (2S,4S)-1-(4-nitrobenzyloxycarbonyl)-2-(piperazin-1-yl)methyl-4-(triphenylmethylthio)pyrrolidine (2.51 g) and triethylamine (0.73 ml) in dichloromethane (25 ml) was added 4-nitrobenzyloxycarbonyl chloride (0.91 g) under ice-cooling and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was washed with saturated aqueous sodium chloride, dried over magnesium sulfate and evaporated in vacuo to give a residue. The residue was chromatographed on silica gel (100 g) eluting with a mixture of dichloromethane and acetone (20:1 V/V). The fractions containing the desired compound were collected and evaporated in vacuo to give (2S,4S)-1-(4-nitrobenzyloxycarbonyl)-2-[4-(4-nitrobenzyloxycarbonyl)piperazin-1-yl]methyl-4-(triphenylmethylthio)pyrrolidine (2.77 g).

1. temperaturecooling
2. washThe reaction mixture was washed with saturated aqueous sodium chloride
3. dry with materialdried over magnesium sulfate
4. customevaporated in vacuo
5. customto give a residue
6. customThe residue was chromatographed on silica gel (100 g)
7. washeluting with a mixture of dichloromethane and acetone (20:1 V/V)
8. additionThe fractions containing the desired compound
9. customwere collected
10. customevaporated in vacuo