反应详情

5h (4.4 g, 11.6 mmol) was suspended in hydrazine hydrate (11 mL) and EtOH (45 mL) and heated to 80° C. overnight. The reaction was cooled to room temperature and concentrated, and then diluted with EtOAc and water. The aqueous layer was extracted with EtOAc twice, and the combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated. The residue was dissolved in CH2Cl2 (15 mL) and heated to dissolve as much of the material as possible. Hexanes (45 mL) was added slowly, and the mixture was stirred for 30 minutes. The precipitate was filtered, rinsed with hexanes, and dried to give the desired product, 5i.

1. concentrationconcentrated
2. additiondiluted with EtOAc and water
3. extractionThe aqueous layer was extracted with EtOAc twice
4. washthe combined organic layers were washed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. dissolutionThe residue was dissolved in CH2Cl2 (15 mL)
9. temperatureheated
10. dissolutionto dissolve as much of the material as possible
11. additionHexanes (45 mL) was added slowly
12. filtrationThe precipitate was filtered
13. washrinsed with hexanes
14. customdried