HRID746143

反应详情

EQUATION

反应方程式

HRID 746143 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6.24 g (0.03 mole) of ethyl 2-chloro-4-methyl-5-thiazolecarboxylate, 4.89 g (0.03 mole) of 2,4-dichlorophenol, 4.14 g (0.03 mole) of potassium carbonate and 40 ml. of acetone was held at reflux for 89 hours. Acetone was removed under reduced pressure. The residue was treated with 50 ml. of water and extracted with ether. The ether solution was washed successively with saturated sodium bicarbonate, 30 ml. of 10% sodium hydroxide and 50 ml. of water. The ether solution was dried (MgSO4) and concentrated. The residue was recrystallized from hexane to give 5.8 g (58%) of ethyl 2-(2',4'-dichlorophenoxy)-4-methyl-5-thiazolecarboxylate as a white solid, m.p. 71°-73° C.

WORKUP

后处理

  1. temperatureat reflux for 89 hours
  2. customAcetone was removed under reduced pressure
  3. additionThe residue was treated with 50 ml
  4. extractionof water and extracted with ether
  5. washThe ether solution was washed successively with saturated sodium bicarbonate, 30 ml
  6. dry with materialThe ether solution was dried (MgSO4)
  7. concentrationconcentrated
  8. customThe residue was recrystallized from hexane