HRID1695581

反应详情

EQUATION

反应方程式

HRID 1695581 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A mixture of 4-methoxy-benzofuran-3-one (CAS 7169-35-9) (30 g, 183 mmol; HPLC 1.241 min), sodium acetate (30.9 g, 375 mmol) and hydroxylamine hydrochloride (5.14 g, 57 mmol) in ethanol (310 ml) was refluxed for 4 h. Cooled to 23° C., filtered the precipitate off, washed with aqueous ethanol and dried in high vacuum to give the title compound as a light red solid (27.74 g, 88%; HPLC 1.448 min); MS (ISP) m/e=180.2 [(M+H)+].

WORKUP

后处理

  1. temperaturewas refluxed for 4 h
  2. filtrationfiltered the precipitate off,
  3. washwashed with aqueous ethanol
  4. customdried in high vacuum