反应详情

温度

0 °C

To a stirred mixture of 3.47 g (15 mmol) of BOC-norleucine (Bachem), 3.44 g (22.5 mmol) of 1-hydroxybenzotriazole monohydrate and 50 mL of dichloromethane at 0° C. was added 3.45 g (1.2 mmol) of EDC. The resulting mixture was stirred at 0° C. for 1 hour and then ammonia gas was bubbled through the mixture for 10 min. The cooling bath was allowed to warm to room temperature and the mixture stirred for 18 hours. The mixture was evaporated at reduced pressure to dryness, triturated with 20% Na2CO3. The resulting solid was collected by filtration and washed with water to yield 2.69 g (11.7 mmol, 78%) of the title compound.

1. customammonia gas was bubbled through the mixture for 10 min
2. temperatureto warm to room temperature
3. stirringthe mixture stirred for 18 hours
4. customThe mixture was evaporated at reduced pressure to dryness
5. customtriturated with 20% Na2CO3
6. filtrationThe resulting solid was collected by filtration
7. washwashed with water