反应详情

A solution of 3,4-dichlorobenzonitrile (2.00 g, 11.6 mmol), hydroxylamine hydrochloride (1.65 mL, 12.8 mmol) and sodium hydroxide (4.15 mL, 12.4 mmol) in ethanol (40 mL) was stirred at rt for 1 h. The reaction mixture was concentrated and refluxed in hexanes for 30 min and concentrated in vacuo. The product, intermediate 33A was used directly without purification. HPLC/MS (Method C) retention time=1.24 min [M+H]+204.9.

1. concentrationThe reaction mixture was concentrated
2. temperaturerefluxed in hexanes for 30 min
3. concentrationconcentrated in vacuo
4. customThe product, intermediate 33A was used directly without purification