HRID1660736

反应详情

EQUATION

反应方程式

HRID 1660736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-trimethylsilylthiazole (135 g, 858 1 mmol) in toluene (1350 mL) add a solution of ethyl chloroformate (98.4 mL, 1.03 mol) in toluene (1350 mL) over 15 min. Stir the reaction at 22° C. for 2 h. Add the solution over aqueous sodium carbonate 25% (wt/wt) (5 L) and stir for 30 min. Separate the organic layer and re-extract the aqueous layer with methylene chloride (2×1 L). Combine the organic layers and evaporate the solvent to provide the title compound (134 g, 99%). ES/MS m/z 158 (M+1)+.

WORKUP

后处理

  1. customthe reaction at 22° C. for 2 h
  2. stirringstir for 30 min
  3. customSeparate the organic layer
  4. extractionre-extract the aqueous layer with methylene chloride (2×1 L)
  5. customCombine the organic layers and evaporate the solvent