反应详情

To a solution of compound 25d (1.1 g, 4.1 mmol) in diethylene glycol (50 mL) was added NH2NH2.H2O (0.28 g, 4.5 mmol). The mixture was refluxed for 2 h and then the water and excess NH2NH2.H2O was removed under vacuum. Then KOH (0.46 g, 8.2 mmol) was added and the mixture was refluxed for 4 h, cooled, diluted with water and extracted with EA. The combined organic layers were washed with brine, dried over Na2SO4, evaporated and purified by prep-TLC to give compound 25e (462 mg, 46%).

1. temperatureThe mixture was refluxed for 2 h
2. customthe water and excess NH2NH2.H2O was removed under vacuum
3. temperaturethe mixture was refluxed for 4 h
4. temperaturecooled
5. extractionextracted with EA
6. washThe combined organic layers were washed with brine
7. dry with materialdried over Na2SO4
8. customevaporated
9. custompurified by prep-TLC