反应详情

To a stirring mixture of the nitro compound 17 (0.96 g, 2.59 mmol) and NiCl2.6H2O (1.24 g, 5.22 mmol) in MeOH/THF (26 mL/39 mL) at 0° C., NaBH4 (0.341 g, 9.01 mmol) was added portion wise. The reaction mixture was stirred for 15 minutes, quenched with 1M HCl (10 mL) and concentrated under reduced pressure to form a green residue, which was then dissolved in 1M HCl (250 mL) and basified with NH4OH. The cloudy suspension was extracted with EtOAc, the organic layer was collected, filtered, washed with water and then dried over anhydrous Na2SO4. Evaporation of this solution afforded title compound 18 as brown solid (0.46 g, 52% yield), which was used in the next step without additional purification. MS (m/z): 341.1 (M+H).

1. customquenched with 1M HCl (10 mL)
2. concentrationconcentrated under reduced pressure
3. customto form a green residue, which
4. extractionThe cloudy suspension was extracted with EtOAc
5. customthe organic layer was collected
6. filtrationfiltered
7. washwashed with water
8. dry with materialdried over anhydrous Na2SO4
9. customEvaporation of this solution