반응 #1551159

반응 방정식

ethyl acetate

hydrazinoacetaldehyde diethyl acetal

methoxyacrylonitrile

→

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

수율 19.3%

용매

water

water

반응 조건

후처리

1. 1
   온도was refluxed for 2 days
2. 2
   온도After the reaction mixture was cooled, to the mixture
3. 3
   workup.ADDITIONwas added
4. 4
   세척The separated organic layer was washed with brine
5. 5
   건조dried over magnesium sulfate
6. 6
   기타The solvent was evaporated
7. 7
   workup.ADDITIONFractions containing the object compound
8. 8
   기타evaporated

실험 절차

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).

출처