反应详情

Compound 111a (1 g, 2.99 mmol) was dissolved in 100 mL of anhydrous tetrahydrofuran and lithium aluminum hydride (342 mg, 8.98 mmol) was added carefully at 0° C. and the mixture was stirred for 30 min. Then, it was refluxed for 3 h and the reaction mixture was poured onto ice portion-wise. It was then filtered and the filtrate was evaporated in vacuo. After addition of 100 mL brine, it was extracted with dichloromethane (100 mL×3). The combined organic layer was dried over Na2SO4, filtered and concentrated to afford 111b as yellow oil (0.6 g, yield 91%)

1. temperatureThen, it was refluxed for 3 h
2. additionthe reaction mixture was poured onto ice portion-wise
3. filtrationIt was then filtered
4. customthe filtrate was evaporated in vacuo
5. additionAfter addition of 100 mL brine, it
6. extractionwas extracted with dichloromethane (100 mL×3)
7. dry with materialThe combined organic layer was dried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated