反应详情

0.24 ml (4.8 mmol) of hydrazine hydrate is added dropwise to 1.00 g (4.08 mmol) of 3-(3-nitro-phenyl)-3-methylmercapto-2-cyano-acrylonitrile in 5.3 ml of methanol and the reaction mixture is then boiled for 1.5 hours. The reaction mixture is then cooled in ice-water and the precipitate is filtered off and washed with diethyl ether/isopropanol (2:1), yielding 5-amino-3-(3-nitro-phenyl)-1H-pyrazole-4-carbonitrile; TLC: Rf =0.4 (methylene chloride:methanol=10:1); TRet (Grad20-100)=10.8; MS: (M)+ =229, (M-NO2)+ =183.

1. filtrationthe precipitate is filtered off
2. washwashed with diethyl ether/isopropanol (2:1)