HRID1445338

反应详情

EQUATION

反应方程式

HRID 1445338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

10.0 g of methyl 3-hydroxy-thiophene-2-carboxylate were dissolved in a mixture of 90 ml of tetrahydrofuran (THF) and 90 ml of methanol, and a solution of 25.2 g of lithium hydroxide in 25 ml of water was added. The reaction mixture was stirred at 22° C. for 18 h and then heated at 55° C. for 6 h. The reaction mixture was concentrated to 50 ml in a rotary evaporator, acidified to pH=1 with 2 molar hydrochloric acid and extracted 3 times with 50 ml of t-butyl methyl ether each time. The combined organic phases were dried over magnesium sulfate and concentrated.

WORKUP

后处理

  1. temperatureheated at 55° C. for 6 h
  2. concentrationThe reaction mixture was concentrated to 50 ml in a rotary evaporator
  3. extractionextracted 3 times with 50 ml of t-butyl methyl ether each time
  4. dry with materialThe combined organic phases were dried over magnesium sulfate
  5. concentrationconcentrated