Preparation method for cyanoethyl graft amide
A technology of grafted amide and cyanoethyl, which is applied in the field of cyanoethyl grafted amide and its preparation, can solve the problems of high reactivity, too fast increase of syrup viscosity, and small dosage, so as to achieve stable reaction process, drug Good slurry flow and leveling, high purity effect
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Embodiment 1
[0021] Dissolve the amide in 4.5 times the volume of dimethyl sulfoxide solvent, add dropwise 2.8 times the molar ratio of propylene under mechanical stirring
[0022] Nitrile, when the acrylonitrile is added dropwise, an ice-water bath is used for cooling, so that the liquid phase temperature is maintained at 30°C. The reaction was carried out at 78°C for 6 hours under reflux and stirring; the reaction was stopped, and excess acrylonitrile and inert solvent were evaporated to obtain a cyanoethyl graft amide.
Embodiment 2
[0024] Dissolve the amide in 4.5 times the volume of a 1:1 mixed solution of dimethyl sulfoxide and acetone, add dropwise 2.5 times the molar ratio of acrylonitrile under mechanical stirring, and use ice-water bath cooling when adding acrylonitrile. Maintain the liquidus temperature at 30°C.
[0025] The reaction was carried out at 50° C. for 12 hours under reflux and stirring; the reaction was stopped, and excess acrylonitrile and inert solvent were evaporated to obtain cyanoethyl graft amide.
Embodiment 3
[0027] Dissolve the amide in 3 times the volume of the dimethyl sulfoxide solution solvent, add 2.2 times the molar ratio of propylene dropwise under mechanical stirring.
[0028] Acrylonitrile, when the acrylonitrile is added dropwise, an ice-water bath is used for cooling, so that the liquid phase temperature is maintained at 27°C. Under reflux and stirring conditions, the reaction was carried out at 100°C for 3 hours; the reaction was stopped, and excess acrylonitrile and inert solvent were evaporated to obtain cyanoethyl graft amide.
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