反应详情

A mixture of compound 65b (1.08 g, 3.11 mmol) and potassium phthalimide (0.634 g) in DMF (10 mL) was stirred at rt overnight. Additional potassium phthalimide (0.063 g) was added and stirring was continued for 4 h. The reaction was diluted with ethyl acetate, washed with water and brine, dried, and concentrated. The residue was dissolved in ethanol (20 mL) and hydrazine (0.34 mL) was added. The reaction mixture was refluxed for 1 h, and then cooled and filtered. The filtrate was concentrated to give compound 65c (1.04 g). ESI-MS m/e 282 (M+1).

1. stirringstirring
2. waitwas continued for 4 h
3. washwashed with water and brine
4. customdried
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in ethanol (20 mL)
7. additionhydrazine (0.34 mL) was added
8. temperatureThe reaction mixture was refluxed for 1 h
9. temperaturecooled
10. filtrationfiltered
11. concentrationThe filtrate was concentrated