HRID2418366

反应详情

EQUATION

反应方程式

HRID 2418366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-oxo-5-chloro-7-(2-chlorophenoxy)indoline (2.0 g.), sodium hydroxide (0.50 g.), dioxane (20 ml.) and water (30 ml.) was refluxed under heating for 23 hours. The reaction mixture was evaporated under reduced pressure and the residue was dissolved in water and filtered. The filtrate was washed with diethyl ether, and diethyl ether was added to the aqueous layer and adjusted to pH 5 with 1N-sulfuric acid. The diethyl ether layer was separated, washed with water, dried over magnesium sulfate and then evaporated. The residue was recrystallized from ethanol to give crystals of 2-[2-amino-3-(2-chlorophenoxy)-5-chlorophenyl]acetic acid (0.725 g.).

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureunder heating for 23 hours
  3. customThe reaction mixture was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in water
  5. filtrationfiltered
  6. washThe filtrate was washed with diethyl ether, and diethyl ether
  7. additionwas added to the aqueous layer and adjusted to pH 5 with 1N-sulfuric acid
  8. customThe diethyl ether layer was separated
  9. washwashed with water
  10. dry with materialdried over magnesium sulfate
  11. customevaporated
  12. customThe residue was recrystallized from ethanol