反应详情

To a solution of 1-{6-[chloro(difluoro)methyl]pyridin-3-yl}ethanone (B) (0.85 g, 4.14 mmol) in MeOH (10 mL) at 0° C. was added NaBH4 (0.16 g, 4.14 mmol). The mixture was stirred for 30 min and 2 M HCl aqueous solution was added until pH reached 7. Solvent was removed under reduced pressure and the remaining mixture was extracted with CH2Cl2 (2×50 mL). The combined organic layer was dried over anhydrous Na2SO4, filtered, concentrated, and dried in vacuo to give 0.798 g of analytically pure 1-{6-[chloro(difluoro)methyl]-pyridin-3-yl}ethanol (C) on GC-MS as a light yellow oil in 93 percent yield. GC-MS: mass calcd for C5H6ClF2NO [M]+ 207. Found 207.

1. customSolvent was removed under reduced pressure
2. extractionthe remaining mixture was extracted with CH2Cl2 (2×50 mL)
3. dry with materialThe combined organic layer was dried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customdried in vacuo