HRID1732180

反应详情

EQUATION

反应方程式

HRID 1732180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of [2,3-dichloro-4-(6-ethyl-3-oxo-1-cyclohexen-1-yl)phenoxy]acetic acid (3.4 g, 0.01 mole), hydroxylamine hydrochloride (2.1 g, 0.03 mole) and pyridine (40 ml) were heated at 95° C. for 40 hours, poured into ice-water and hydrochloric acid, extracted with ether, washed with water, dried over magnesium sulfate and evaporated in vacuo. After recrystallization from toluene (120 ml) the [2,3-dichloro-4-(6-ethyl-3-(hydroxyimino)-1-cyclohexen-1-yl)-phenoxy]acetic acid hemitoluene solvate melted at 88°-90° C.

WORKUP

后处理

  1. extractionextracted with ether
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customAfter recrystallization from toluene (120 ml) the [2,3-dichloro-4-(6-ethyl-3-(hydroxyimino)-1-cyclohexen-1-yl)-phenoxy]acetic acid hemitoluene solvate melted at 88°-90° C.