反应详情

Sodium hydride (470 mg. of 50% in oil, 0.011 mole) is added to a slurry of ethyl 7,8-dimethoxypyrimido[4,5-b]quinolin-4(3H)-one-2-carboxylate (3.3 g., 0.01 mole) in N,N-dimethylformamide (75 ml.). The mixture is stirred and heated on a steambath for 10 minutes and then at room temperature for a half hour. It is cooled in an ice-bath and iodomethane (2.19 g., 0.015 mole) added dropwise over a 30 minute period. Following completion of addition, the mixture is stirred for an additional 15 minutes in an ice-bath and then for a half-hour at room temperature. The reaction mixture is poured into ice-water (200 ml.) and the resulting solid filtered off, air-dried, and recrystallized from ethanol to give 2.1 g. of yellow crystals (61.2%); m.p. 211.5° C. (dec.)

1. temperatureheated on a steambath for 10 minutes
2. waitat room temperature for a half hour
3. temperatureIt is cooled in an ice-bath
4. additioncompletion of addition
5. stirringthe mixture is stirred for an additional 15 minutes in an ice-bath
6. waitfor a half-hour at room temperature
7. filtrationthe resulting solid filtered off
8. customair-dried
9. customrecrystallized from ethanol
10. customto give 2.1 g