反应详情

mf) A solution of 31.18 g of ethyl 2-(2-chloro-4-iodo-benzoyl)-3-ethoxy-acrylate in 500 ml of methylene chloride is treated dropwise with 7.95 g of cyclohexylamine while cooling with ice and stirring. After 6 hrs. at room temperature the reaction mixture is concentrated and, for crystallization, the residue is stirred with 200 ml of hexane. The precipitate is filtered off under suction, washed with 100 ml of hexane and dried. 19.2 g (55%) of ethyl 2-(2-chloro-4-iodo-benzoyl)-3-cyclohexylamino-acrylate are obtained as a colourless solid. M.p. 154°-156° C.

1. temperaturewhile cooling with ice
2. concentrationat room temperature the reaction mixture is concentrated and, for crystallization
3. stirringthe residue is stirred with 200 ml of hexane
4. filtrationThe precipitate is filtered off under suction
5. washwashed with 100 ml of hexane
6. customdried