反应详情

Sodium hydride (0.9 g of a 50% dispersion in mineral oil) was added to a solution of N-(2-bromo-6-methoxy-3-pyridinyl)-2-ethylamino-N-methyl-3-pyridinecarboxamide (1.4 g) in xylene (20 ml) and the mixture refluxed for 2 hours. After cooling, the mixture was quenched with methanol, diluted with ethyl acetate, and washed with water. The organic phase was dried (anhydrous magnesium sulfate), concentrated, and purified on a silica gel column (ethyl acetate/hexane, 1:4) to give fairly pure product, which was then recrystallized twice from ethyl acetate/hexane to give 0.52 g of pure 5,11-dihydro-11-ethyl-2-methoxy-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 116°-118° C.

1. temperaturethe mixture refluxed for 2 hours
2. temperatureAfter cooling
3. customthe mixture was quenched with methanol
4. additiondiluted with ethyl acetate
5. washwashed with water
6. dry with materialThe organic phase was dried (anhydrous magnesium sulfate)
7. concentrationconcentrated
8. custompurified on a silica gel column (ethyl acetate/hexane, 1:4)
9. customto give fairly pure product, which
10. customwas then recrystallized twice from ethyl acetate/hexane