反应详情

To a stirred suspension of lithium aluminum hydride (LAH, 7.0 g) in 250 mL of ether is added dropwise a solution of the compound of step 1(10.0 g) in 10 mL of ether at −70° C. The reaction mixture is stirred at −60° C. to −70° C. until TLC (10% MeOH in CH2Cl2) shows the disappearance of the starting material. The excess LAH is destroyed by cautious addition of a saturated aqueous Na2SO4 solution. The resulting mixture is filtered and solid is washed with EtOAc. The filtrate is dried over Na2SO4 and concentrated under vacuum to give 8.3 g of the title compound as clear oil.

1. customThe excess LAH is destroyed by cautious addition of a saturated aqueous Na2SO4 solution
2. filtrationThe resulting mixture is filtered
3. washsolid is washed with EtOAc
4. dry with materialThe filtrate is dried over Na2SO4
5. concentrationconcentrated under vacuum