反应详情

温度

-10 °C

To 100 mL (0.10 mol) of 1.0 M BnMgBr in THF 9.50 g (90 mmol) of benzaldehyde (2) was added with vigorous stirring at −10° C. This mixture was slowly warmed to room temperature and then stirred for 2 hr at this temperature. The mixture was added to 300 mL of saturated aqueous Na2SO4. The organic layer was separated and washed with saturated aqueous NH4Cl. The aqueous layer was extracted with 2×100 mL of diethyl ether. The combined organic extracts were evaporated to dryness, and the residue was dissolved in 100 mL of dichloromethane. The obtained solution was dried over Na2SO4 and evaporated to dryness. This crude product was further used without an additional purification. Yield 12.0 g (67%) of the title compound.

1. temperatureThis mixture was slowly warmed to room temperature
2. stirringstirred for 2 hr at this temperature
3. customThe organic layer was separated
4. washwashed with saturated aqueous NH4Cl
5. extractionThe aqueous layer was extracted with 2×100 mL of diethyl ether
6. customThe combined organic extracts were evaporated to dryness
7. dissolutionthe residue was dissolved in 100 mL of dichloromethane
8. dry with materialThe obtained solution was dried over Na2SO4
9. customevaporated to dryness
10. customThis crude product was further used without an additional purification