反应详情

With the exclusion of air, 7.22 g (42.4 mmol) of 3,3-bis(methylsulfanyl)-2-cyano-acrylonitrile (Maybridge), 7.90 g (42.4 mmol) of piperazine-N-carboxylic acid tert-butyl ester (Aldrich; Milwaukee/USA) and 0.24 g (3 mmol) of pyridine are heated to boiling in 75 ml of isopropanol for 4 hours. Cooling, concentration by evaporation and drying under a high vacuum yield 3-(4-tert-butoxycarbonyl-piperazin-1-yl)-3-methylsulfanyl-2-cyano-acrylonitrile; C14H20N4SO2: calc. C54.52%, H 6.54%, N 18.17%, S 10.40%; found C54.37%, H 6.50%, N 17.85%, S 10.25%.

1. temperatureCooling
2. concentrationconcentration
3. customby evaporation
4. customdrying under a high vacuum