反应详情

3.10 g of trans-1-(p-nitrobenzyloxycarbonyl)-4-hydroxy-L-proline and 1.10 g of triethylamine were dissolved in 40 ml of dried tetrahydrofuran, and a solution of 1.20 g of ethyl chloroformate in 10 ml of dried tetrahydrofuran was added dropwise thereto at -25° C. to -35° C. After stirring at the same temperature for 50 minutes, 10 ml of concentrated aqueous ammonia was added dropwise to the mixture at -25° to -40° C. The temperature was then gradually elevated to room temperature, and the reaction mixture was stirred for 1 hour, followed by concentration under reduced pressure. To the residue were added 20 ml of water and 50 ml of diethyl ether. After ice-cooling, the thus formed white crystals were separated by filtration, washed successively with cool water and cool diethyl ether, and dried under reduced pressure to yield trans-1-(p-nitrobenzyloxycarbonyl)-4-hydroxy-L-prolineamide.

1. customat -25° C. to -35° C
2. customwas then gradually elevated to room temperature
3. stirringthe reaction mixture was stirred for 1 hour
4. concentrationfollowed by concentration under reduced pressure
5. additionTo the residue were added 20 ml of water and 50 ml of diethyl ether
6. temperatureAfter ice-cooling
7. customthe thus formed white crystals were separated by filtration
8. washwashed successively with cool water
9. temperaturecool diethyl ether
10. customdried under reduced pressure