反应详情

温度

0 °C

To a stirred solution of 4-(2-oxo-2H-pyridin-1-yl)-benzoic acid (0.31 g, 1.4 mmol) in THF (12 mL) was added Et3N (0.30 mL, 2.15 mmol, 1.5 eq) followed by dropwise addition of ClCOOEt (0.16 mL, 1.2 eq) at 0° C. under N2. The mixture was stirred for 1 h at 0° C., filtered, and rinsed with THF. The THF solution was stirred at 0° C., MeOH (3 mL) was added followed by portionwise addition of NaBH4 (0.26 g, 6.8 mmol). The mixture was stirred at 0° C. for 20 min, sat'd Na2SO4 added, extracted with CH2Cl2, dried (MgSO4), filtered, and concentrated to dryness to give 4-(2-oxo-2H-pyridin-1-yl)-benzaldehyde (0.17 g) as a tan solid.

1. filtrationfiltered
2. washrinsed with THF
3. stirringThe THF solution was stirred at 0° C.
4. additionMeOH (3 mL) was added
5. stirringThe mixture was stirred at 0° C. for 20 min
6. additionadded
7. extractionextracted with CH2Cl2
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated to dryness