反应详情

A solution of sodium dithionite (94 g, 0.54 mol) in water (1 L) was added to a stirred mixture of 3-amino-5,6-dichloro-2-nitrotoluene (from step (b), 39.7 g, 0.18 mol) and potassium bicarbonate (94 g, 0.94 mmol) in methanol (1 L) at room temperature. After 30 minutes, the mixture was concentrated under reduced pressure and the resulting suspension extracted with ethyl acetate (total of 700mi). The extracts were dried (MgSO4) and concentrated under reduced pressure to give 2,3-diamino-5,6-dichlorotoluene (26.1 g, 38% over 2 steps) as a brown solid.

1. concentrationthe mixture was concentrated under reduced pressure
2. extractionthe resulting suspension extracted with ethyl acetate (total of 700mi)
3. dry with materialThe extracts were dried (MgSO4)
4. concentrationconcentrated under reduced pressure