HRID1265624

反应详情

EQUATION

反应方程式

HRID 1265624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of rac-3-(2-bromo-propionyl)-benzoic acid methyl ester (2.71 g) and 2-(tert.-butylcarbonyloxy)thioacetamide (2.1 g) in EtOH (20 mL) was heated at reflux for 6 h. The mixture was partitioned between AcOEt and brine, and the organic layer was dried and evaporated. A solution of the residual oil and NaOMe (0.54 g) in MeOH (20 mL) was stirred at 60° C. for 1 h. The solution was diluted with AcOEt, washed with 1N HCl and brine, dried and evaporated to give 3-(2-hydroxymethyl-5-methyl-thiazol-4-yl)-benzoic acid methyl ester (1.17 g) as white crystals, MS (ISP) 264.1 [(M+H)+].

WORKUP

后处理

  1. temperatureat reflux for 6 h
  2. customThe mixture was partitioned between AcOEt and brine
  3. customthe organic layer was dried
  4. customevaporated
  5. additionThe solution was diluted with AcOEt
  6. washwashed with 1N HCl and brine
  7. customdried
  8. customevaporated