反应 #1673835

反应方程式

ethyl acetate

hydrazinoacetaldehyde diethyl acetal

methoxyacrylonitrile

→

1-(2,2-diethoxyethyl)-5-aminopyrazole

收率 19.3%

溶剂

water

water

反应条件

后处理

1. 1
   温度was refluxed for 2 days
2. 2
   温度After the reaction mixture was cooled, to the mixture
3. 3
   workup.ADDITIONwas added
4. 4
   洗涤The separated organic layer was washed with brine
5. 5
   干燥dried over magnesium sulfate
6. 6
   其他The solvent was evaporated
7. 7
   workup.ADDITIONFractions containing the object compound
8. 8
   其他evaporated

实验过程

A mixture of hydrazinoacetaldehyde diethyl acetal (21 g) and methoxyacrylonitrile (11.8 g) in water (150 ml) was refluxed for 2 days. After the reaction mixture was cooled, to the mixture was added a mixture of water and ethyl acetate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was evaporated and the residue was subjected to column chromatography on silica gel using ethyl acetate as an eluent. Fractions containing the object compound were combined and evaporated to give 1-(2,2-diethoxyethyl)-5-aminopyrazole (5.45 g).

来源