反应详情

A mixture of 4-cyanobenzaldehyde (3.3 g, 25.2 mmol), N-methylhydroxyamine hydrogen chloride and sodium bicarbonate (4.23 g, 50.4 mmol) in dry methylene chloride (80 ml) was stirred at rt for 5 hrs. The solid portion was filtered off and the filtrate was concentrated to give the product as white solid (98% yield). 1H NMR (300 MHz, CDCl3) δ3.94(s, 3H), 7.46(s, 1H), 7.72(d, J=8 Hz, 2H), 8.32(d, J=8 Hz, 2H). MS (NH3-CI) Calc. for (M+1)+: 161. Found: 161.

1. filtrationThe solid portion was filtered off
2. concentrationthe filtrate was concentrated