反应详情

温度

70 °C

2-Chloro-5-nitrobenzonitrile (25 g, 137 mmol) was dissolved in ethanol (275 mL). Stannous chloride dihydrate (154.5 g, 0.685 M) was added and the mixture stirred at 70° C. for 30 min. The mixture was then cooled to room temperature and poured into crushed ice. The mixture was made basic with solid sodium hydroxide. This mixture was extracted with ethyl acetate (3×100 mL). The extracts were combined, washed with brine, dried (MgSO4), concentrated and the residue dried under vacuum and recrystallized from ethanol to yield light brown needles (10.6 g, 51%).

1. temperatureThe mixture was then cooled to room temperature
2. additionpoured
3. custominto crushed ice
4. extractionThis mixture was extracted with ethyl acetate (3×100 mL)
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customthe residue dried under vacuum
9. customrecrystallized from ethanol