Reacción #1673835

Ecuación de reacción

ethyl acetate

hydrazinoacetaldehyde diethyl acetal

methoxyacrylonitrile

→

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

Rendimiento 19.3%

Disolventes

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas refluxed for 2 days
2. 2
   TemperaturaAfter the reaction mixture was cooled, to the mixture
3. 3
   workup.ADDITIONwas added
4. 4
   LavadoThe separated organic layer was washed with brine
5. 5
   Secadodried over magnesium sulfate
6. 6
   OtroThe solvent was evaporated
7. 7
   workup.ADDITIONFractions containing the object compound
8. 8
   Otroevaporated

Procedimiento

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).

Fuente