HRID1266771

反应详情

EQUATION

反应方程式

HRID 1266771 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 methyl 3-(2-bromo-propionyl)-benzoate (2.7 g) and 2-(tert.-butyl-carbonyloxy)thioacetamide (2.1 g) in EtOH (20 mL) was heated at reflux for 8 h. The mixture was partitioned between H2O and AcOEt. The organic layer was dried and evaporated. The residue was dissolved in MeOH (20 ml), NaOMe (0.54 g) was added, and the mixture was heated to 60° C. for 1 h. The mixture was diluted with AcOEt and then washed with 3N HCl and brine. The organic layer was dried and evaporated and the residue was crystallized from AcOEt to give methyl 3-[2-hydroxymethyl-5-methyl-thiazol-4-yl]-benzoate (1.17 g) as white solid.

WORKUP

后处理

  1. temperatureat reflux for 8 h
  2. customThe mixture was partitioned between H2O and AcOEt
  3. customThe organic layer was dried
  4. customevaporated
  5. dissolutionThe residue was dissolved in MeOH (20 ml)
  6. additionNaOMe (0.54 g) was added
  7. additionThe mixture was diluted with AcOEt
  8. washwashed with 3N HCl and brine
  9. customThe organic layer was dried
  10. customevaporated
  11. customthe residue was crystallized from AcOEt