HRID2117908

反应详情

EQUATION

反应方程式

HRID 2117908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 3-bromo-2-oxo-4-phenylbutanoate (5.8 g) was dissolved in EtOH (110 ml), and then thiourea (3.1 g) was added to the solution. The reaction mixture was refluxed for 2 hours under N2 atmosphere. The cooled reaction mixture was evaporated in vacuo. The residual solid was suspended (pH=8) in saturated NaHCO3 and water. The solid was collected by filtration, and purified by flash column chromatography over silica gel with CHCl3/MeOH (10:1) as an eluent to give ethyl 2-amino-5-benzyl-1,3-thiazole-4-carboxylate (808.2 mg) as a yellow wax.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 2 hours under N2 atmosphere
  2. customThe cooled reaction mixture
  3. customwas evaporated in vacuo
  4. filtrationThe solid was collected by filtration
  5. custompurified by flash column chromatography over silica gel with CHCl3/MeOH (10:1) as an eluent