反応 #1551159

反応方程式

ethyl acetate

hydrazinoacetaldehyde diethyl acetal

methoxyacrylonitrile

→

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

収率 19.3%

溶媒

water

water

反応条件

後処理

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
   洗浄The separated organic layer was washed with brine
5. 5
   乾燥dried over magnesium sulfate
6. 6
   その他The solvent was evaporated
7. 7
   workup.ADDITIONFractions containing the object compound
8. 8
   その他evaporated

実験手順

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).

出典