HRID1834670

反应详情

EQUATION

反应方程式

HRID 1834670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[2-Chloro-4-(2-dimethylaminomethylbutyryl)phenyoxy]acetic acid hydrochloride (8.7 g., 0.025 mole), water (100 ml.), and saturated aqueous sodium bicarbonate (100 ml.) are combined and heated on a steam bath for 2.5 hours. The reaction mixture is acidified, extracted with ether and dried over magnesium sulfate. Distillation of the solvent at reduced pressure leaves 1.3 g. (20%) of [2-chloro-4-(2-methylenebutyryl)phenoxy]acetic acid which melts at 83.5°-85.5° C. after recrystallization from methyl cyclohexane (75 ml.).

WORKUP

后处理

  1. temperatureheated on a steam bath for 2.5 hours
  2. extractionextracted with ether
  3. dry with materialdried over magnesium sulfate
  4. distillationDistillation of the solvent at reduced pressure
  5. customleaves 1.3 g
  6. custom(20%) of [2-chloro-4-(2-methylenebutyryl)phenoxy]acetic acid which melts at 83.5°-85.5° C. after recrystallization from methyl cyclohexane (75 ml.)