反应详情

Lithium aluminum hydride was added to 100 ml THF and stirred for 10 minutes and cooled in an ice bath. A solution of Compound 69A (9.06 g, 33.4 mmol) in 200 ml THF was added dropwise over ½ hr to the lithium aluminum hydride solution and stirred for 2 h. A saturated solution of water/sodium sulfate decahydrate was added until gas evolution ceased and a heavy white precipitate formed. The reaction was stirred for 30 minutes more and filtered through Celite®, extracted into 2×200 ml ethyl acetate, washed with 1×50 ml brine dried over anhydrous sodium sulfate, and filtered through silica. The product was eluted with 300 ml ethyl acetate and concentrated to give a cream colored solid. MS m/z 244 (M+1).

1. temperaturecooled in an ice bath
2. stirringstirred for 2 h
3. customa heavy white precipitate formed
4. stirringThe reaction was stirred for 30 minutes more
5. filtrationfiltered through Celite®
6. extractionextracted into 2×200 ml ethyl acetate
7. washwashed with 1×50 ml brine
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationfiltered through silica
10. washThe product was eluted with 300 ml ethyl acetate
11. concentrationconcentrated
12. customto give a cream