反应详情

温度

-78 °C

To a stirred solution of 6-tert-Butyldimethylsilyloxy-2,3-dihydrobenzofuran-3-one (42 g, 158 mmol) in dichloromethane (1.4 L) at −78° C. under nitrogen was slowly added a solution of DIBAL-H (238 mL, 1.0 M, 238 mmol) in dichloromethane. The reaction was stirred at −78° C. for 1 h, and then was quenched carefully with ethyl acetate (1.0 L). Cold bath was removed, and a solution of Rochelle's salt (400 mL, 10%) was added continuously with stirring over a period of 2 h. The mixture was then diluted with MTBE (4.0 L), washed with brine, dried with magnesium sulfate, filtered and concentrated to yield the final product as yellow oil.

1. customwas quenched carefully with ethyl acetate (1.0 L)
2. customCold bath was removed
3. additiona solution of Rochelle's salt (400 mL, 10%) was added continuously
4. stirringwith stirring over a period of 2 h
5. additionThe mixture was then diluted with MTBE (4.0 L)
6. washwashed with brine
7. dry with materialdried with magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated