HRID1835331

反应详情

EQUATION

反应方程式

HRID 1835331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.20 g (10.8 mmol) 6-chloro-4-(2-chloro-phenyl)-nicotinic acid ethyl ester, 50 ml dioxane and 50 ml of a 2 M aqueous sodium hydroxide solution was stirred at room temperature for 17 h. Dilution with water was followed by washing with two portions of tert-butyl methyl ether. The combined organic layers were extracted with 1 M aqueous sodium hydroxide solution. The combined aqueous layers were acidified to pH 2 with 2 M aqueous hydrochloric acid solution and extracted with four portions of tert-butyl methyl ether. The combined organic extracts were dried with sodium sulfate and concentrated to give 2.90 g (100%) of the title compound as an off-white solid.

WORKUP

后处理

  1. washby washing with two portions of tert-butyl methyl ether
  2. extractionThe combined organic layers were extracted with 1 M aqueous sodium hydroxide solution
  3. extractionextracted with four portions of tert-butyl methyl ether
  4. dry with materialThe combined organic extracts were dried with sodium sulfate
  5. concentrationconcentrated