反应详情

BH3/THF (279 mL; 279 mmol) was added to a solution of 4-chloro-3-nitrobenzonitrile (30 g; 164 mmol) in THF (100 mL) over 30 min at 0° C. and the resulting mixture was stirred over night and allowed to reach rt. MeOH (150 mL) and conc. HCl (60 mL) was added and the resulting mixture was refluxed for 4 h and thereafter concentrated. The residue was treated with water (500 mL) and the resulting precipitate was filtered off. The filtrate was treated with NaCl (120 g) and heated and the resulting precipitate was filtered off to give the sub-title compound. Yield: 24.059 g (65%).

1. customto reach rt
2. temperaturethe resulting mixture was refluxed for 4 h
3. concentrationconcentrated
4. additionThe residue was treated with water (500 mL)
5. filtrationthe resulting precipitate was filtered off
6. additionThe filtrate was treated with NaCl (120 g)
7. temperatureheated
8. filtrationthe resulting precipitate was filtered off