反应详情

温度

5 °C

N-Hydroxysuccinimide (25.3 g) was added to a solution of 1-(t-butoxycarbonyl)piperidine-4-carboxylic acid (45.8 g) in DMF (250 ml) and the mixture stirred at 5° C. EDAC (42 g) was added and the mixture stirred for 4 hours at 5° C. A further portion of EDAC (5.73 g) was added and the mixture allowed to warm to ambient temperature and stirred overnight. The mixture was evaporated to half its original volume and the residue partitioned between ethyl acetate (1000 ml) and water (250 ml). The ethyl acetate phase was separated, washed with water (2×250 ml), brine (50 ml), dried (MgSO4) and evaporated to give a solid which was recrystallised from a mixture of ethyl acetate/hexane (250 ml/500 ml) to give 1-(1-(t-butoxycarbonyl)piperidin-4-ylcarbonyloxy)2,5-dioxopyrrolidine (55 g);

1. stirringthe mixture stirred for 4 hours at 5° C
2. temperatureto warm to ambient temperature
3. stirringstirred overnight
4. customThe mixture was evaporated to half its original volume
5. customthe residue partitioned between ethyl acetate (1000 ml) and water (250 ml)
6. customThe ethyl acetate phase was separated
7. washwashed with water (2×250 ml), brine (50 ml)
8. dry with materialdried (MgSO4)
9. customevaporated
10. customto give a solid which
11. customwas recrystallised from a mixture of ethyl acetate/hexane (250 ml/500 ml)