Reaktion #1673835

Reaktionsgleichung

ethyl acetate

hydrazinoacetaldehyde diethyl acetal

methoxyacrylonitrile

→

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

Ausbeute 19.3%

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 2 days
2. 2
   TemperaturAfter the reaction mixture was cooled, to the mixture
3. 3
   workup.ADDITIONwas added
4. 4
   WaschenThe separated organic layer was washed with brine
5. 5
   Trocknendried over magnesium sulfate
6. 6
   SonstigeThe solvent was evaporated
7. 7
   workup.ADDITIONFractions containing the object compound
8. 8
   Sonstigeevaporated

Vorschrift

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).

Quelle