反应详情

A mixture of 102.1 g (600 mmol) of 3,3-bis-methylmercapto-2-cyano-acrylonitrile, 133.3 g (600 mmol) of 3-(N-Boc-aminomethyl)-aniline (WO 93/00095) and 1100 ml of methanol is heated under reflux for 6.5 hours and then concentrated by evaporation in vacuo. Crystallization of the residue from ethyl acetate, filtration and washing the filtration residue with ethyl acetate yield 3-[3-(N-Boc-aminomethyl)-phenylamino]-2-cyano-3-methylmercapto-acrylonitrile; m.p. 150-151° C.

1. temperatureis heated
2. temperatureunder reflux for 6.5 hours
3. concentrationconcentrated by evaporation in vacuo
4. customCrystallization of the residue
5. filtrationfrom ethyl acetate, filtration
6. washwashing the filtration residue with ethyl acetate