HRID542104

反应详情

EQUATION

反应方程式

HRID 542104 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl 2,6-bis(trifluoromethyl)-4-hydroxy-3-pyridinecarboxylate (product of Example 3, 15 g, 0.0495 mol) in 5% aqueous sodium hydroxide (60 ml, 0.148 mol) was refluxed for 3 hours. The reaction was complete as judged by TLC (10% methanol in ethyl acetate). The mixture was then poured into a mixture of ice in concentrated aqueous hydrochloric acid and extracted with ethyl acetate. The ethyl acetate solution was dried over magnesium sulfate, and concentrated to give a light brown solid (13 g). It was treated with petroleum ether to give 11.9 g of a white solid (83%); mp 168°-172° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe ethyl acetate solution was dried over magnesium sulfate
  3. concentrationconcentrated