反应详情

To a solution of 3-nitrobenzaldehyde (1) (200 g, 1.32 mol) in methanol (1000 mL) at 0° C. under N2 atmosphere was slowly added NaBH4 (25 g, 0.66 mol) and then the reaction mixture was allowed to stir at room temperature for 1 h. The reaction mixture was re-cooled to 0° C. and quenched with ice-water, methanol was removed under reduced pressure and the residue was extracted with CH2Cl2 (5×200 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and concentrated to furnish compound 2 (190.7 g, 93%) as liquid which was taken as such for next step.

1. customat 0° C.
2. temperatureThe reaction mixture was re-cooled to 0° C.
3. customquenched with ice-water, methanol
4. customwas removed under reduced pressure
5. extractionthe residue was extracted with CH2Cl2 (5×200 mL)
6. washThe combined organic layer was washed with brine
7. dry with materialdried over anhydrous Na2SO4
8. concentrationconcentrated