反应详情

Title product of Example A3 (0.3 g, 1.0 mmole), morpholine (0.45 ml, 5 mmole) and ethanol (10 ml) were combined and stirred 18 hours at 25°. Additional morpholine (2 ml) was added and the mixture refluxed 4 hours. The reaction mixture was evaporated in vacuo to an oil, chromatographed on silica gel (4.5 cm×18 cm) eluting with ethyl acetate, initially isolating purified title product as an oil which crystallized on standing under ether/pentane, 0.27 g; m.p. 130°-132.5° C.

1. temperaturethe mixture refluxed 4 hours
2. customThe reaction mixture was evaporated in vacuo to an oil
3. customchromatographed on silica gel (4.5 cm×18 cm)
4. washeluting with ethyl acetate
5. custominitially isolating
6. custompurified title product as an oil which
7. customcrystallized