HRID2363750
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- concentrationThe reaction mixture is concentrated to less than 20% of its initial volume
- additiondiluted with 20 mL of water
- additionSolid sodium carbonate is added at 0-5° C.
- customto obtain a pH of 8-9
- filtrationThe precipitate is filtered off by suction
- custompurified by chromatography on silica
- washeluting with a mixture of dichloromethane and methanol (98/2)