HRID509450

反应详情

EQUATION

反应方程式

HRID 509450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3-methoxy-4-nitrobenzaldehyde (53.5 g, 295.5 mmol)) in EtOH (285 ml) was slowly added a solution of hydroxylamine hydrochloride (30.8 g, 443 mmol) in water (50 ml). The reaction mixture was stirred overnight, poured into ice-cold water, and the formed precipitate was collected by filtration to furnish 44 g of 3-methoxy-4-nitrobenzaldehyde oxime. The filtrate was extracted with DCM, and the organic phase was washed with water and brine, dried over sodium sulfate, and concentrated to furnish additional 8.2 g of the title product. 1H NMR (CDCl3) δ: 8.13 (s, 1H), 7.87 (d, J=8.2 Hz, 1H), 7.51 (s, 1H), 7.35 (s, 1H), 7.18 (dd, J=8.4, 1.4 Hz, 1H), 4.01 (s, 3H).

WORKUP

后处理

  1. additionpoured into ice-cold water
  2. filtrationthe formed precipitate was collected by filtration