反应详情

To a solution of 5-chlorophthalide (3.64 g, 21.6 mmol) in dichloromethane (100 mL) at −78° C. was added di-isobutylaluminium hydride (1M in toluene) (23.8 mL, 23.8 mmol) dropwise. After 1 h the reaction mixture was quenched with a saturated solution of sodium tartrate (250 mL), allowed to warm to room temperature and stirred for 1 h. The layers were separated and the aqueous layer extracted with dichloromethane. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo to yield the title compound as a white solid.

1. customAfter 1 h the reaction mixture was quenched with a saturated solution of sodium tartrate (250 mL)
2. customThe layers were separated
3. extractionthe aqueous layer extracted with dichloromethane
4. dry with materialThe combined organic layers were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo