HRID2363750

反应详情

EQUATION

反应方程式

HRID 2363750 的结构方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A suspension of 580 mg of ethyl 6-[hydrazino(imino)methyl]imidazo[1,2-a]pyridine-2-carboxylate in 6 mL of formic acid is heated for 20 hours at 85° C. The reaction mixture is concentrated to less than 20% of its initial volume and diluted with 20 mL of water. Solid sodium carbonate is added at 0-5° C. to obtain a pH of 8-9. The precipitate is filtered off by suction, and then purified by chromatography on silica, eluting with a mixture of dichloromethane and methanol (98/2) to give 320 mg of ethyl 6-(1H-1,2,4-triazol-3-yl)imidazo[1,2-a]pyridine-2-carboxylate.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated to less than 20% of its initial volume
  2. additiondiluted with 20 mL of water
  3. additionSolid sodium carbonate is added at 0-5° C.
  4. customto obtain a pH of 8-9
  5. filtrationThe precipitate is filtered off by suction
  6. custompurified by chromatography on silica
  7. washeluting with a mixture of dichloromethane and methanol (98/2)