HRID972237

反应详情

EQUATION

反应方程式

HRID 972237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 2.8 g of crude 2-methyl-4-(6-carbomethoxyhexyl)-5-hydroxymethyl thiazole (XII, R1 = CH3) in 25 ml of dichloromethane was dropwise added to the solution of 16 g of chromium trioxide-dipyiridine complex in 320 ml of dichloromethane. Stirring of the reaction mixture was continued for 30 minutes, then the reaction mixture was filtered and the filtrate was evaporated in vacuo. After purifying the crude product obtained as evaporation residue, by preparative thin layer chromatography using a silica gel layer as adsorbent and a mixture of 50 % ethyl acetate and 50 % of n-heptane as running solvent, 2.15 g of 2-methyl-4-(6-carbomethoxyhexyl)-thiazole-5-carbaldehyde (XIII, R1 = CH3) were obtained.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. customthe filtrate was evaporated in vacuo
  3. customAfter purifying the crude product
  4. customobtained as evaporation residue, by preparative thin layer chromatography