反应详情

温度

70 °C

To a solution of 4-azido-N-ethylbenzamide (1.00 g) obtained in Example 43a) and methyl 3-oxoheptanoate (1.10 g) in methanol (50 ml) was added a solution of sodium methoxide in methanol (1.35 g, 28%). The reaction mixture was stirred at room temperature for 8 hr and at 70° C. for 3 hr, and 1M aqueous sodium hydroxide solution (11 ml) was added. The reaction mixture was stirred at 70° C. for 1 hr, cooled to room temperature, diluted with water, and methanol was evaporated under reduced pressure. The residual aqueous solution was acidified (pH=1) with 1M hydrochloric acid under ice-cooling, the insoluble material was collected by filtration and washed with water to give the title compound as a brown powder (1.66 g, 99%).

1. stirringThe reaction mixture was stirred at 70° C. for 1 hr
2. temperaturecooled to room temperature
3. customwas evaporated under reduced pressure
4. temperaturecooling
5. filtrationthe insoluble material was collected by filtration
6. washwashed with water