反応 #1551173

反応方程式

hydrazinoacetaldehyde diethyl acetal

ethoxymethylenemalononitrile

→

5-amino-4-cyano-1-(2,2-diethoxyethyl)pyrazole

収率 30.2%

溶媒

ethanol

ethanol

反応条件

後処理

1. 1
   その他The reaction mixture was evaporated in vacuo
2. 2
   workup.ADDITIONTo the residue was added diethyl ether (400 ml)
3. 3
   ろ過the resultant precipitate was filtered off
4. 4
   workup.ADDITIONa mixture of ethyl acetate and hexane (2:3) as an eluent
5. 5
   workup.ADDITIONFractions containing the object compound
6. 6
   その他evaporated

実験手順

To a solution of hydrazinoacetaldehyde diethyl acetal (52.6 g) in ethanol (110 ml) was added dropwise a solution of ethoxymethylenemalononitrile (41.5 g) in ethanol (420 ml) at room temperature. The mixture was stirred at ambient temperature for 24 hours. The reaction mixture was evaporated in vacuo. To the residue was added diethyl ether (400 ml) and the resultant precipitate was filtered off. The filtrate was subjected to column chromatography on silica gel using a mixture of ethyl acetate and hexane (2:3) as an eluent. Fractions containing the object compound were combined and evaporated to give 5-amino-4-cyano-1-(2,2-diethoxyethyl)pyrazole (23.0 g).

出典