HRID1660568

反应详情

EQUATION

反应方程式

HRID 1660568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Utilizing the procedure of Example 1, a mixture of 1.97 g (0.01 mol) of ethyl 2-chloro-4-methyl-pentanoate, 0.76 g (0.01 mol) of thiourea and 30 ml of ethanol was held at reflux for 18 hours. Ethanol was removed under reduced pressure. The residue was crystallized from hexane. The solid precipitates were dissolved in ether. The ether solution was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from benzene-ether to give 0.85 g (39.6%) of ethyl 2-amino-4-isopropyl-5-thiazolecarboxylate, m.p. 173°-176° C.

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. customEthanol was removed under reduced pressure
  3. customThe residue was crystallized from hexane
  4. customThe solid precipitates
  5. dissolutionwere dissolved in ether
  6. washThe ether solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was recrystallized from benzene-ether