| production method | the synthesis of chloride has two kinds: phosgene route and non-phosgene route. The phosgene route is the reaction of N-methylaniline with phosgene to produce N-methyl-N-phenylcarbamoyl chloride, which is further chlorinated on the N-methyl group to obtain the desired chloride. The carbon tetrachloride was pumped into the actinic reaction kettle, and N-methylaniline and carbon tetrachloride were pumped into the N-methylaniline dropping tank for standby. When heated to 40 ° C., phosgene was continuously introduced, and N-methylaniline carbon tetrachloride solution was added dropwise at the same time, and the dropping acceleration was limited to no precipitation. After the dropwise addition, the phosgene was stopped, cooled to room temperature, and the excess of phosgene was driven by nitrogen to obtain N-methyl-N-phenylcarbamoyl chloride carbon tetrachloride solution. The solution was added to the chlorination reaction kettle, and chlorine was introduced after irradiation with UV light at 20 ℃ for 0.5H. With the exotherm of the reaction, the temperature gradually increased, and the reaction lasted for about 2-4H. When the reaction solution began to cool down, it was cooled to 20 ° C. And chlorine gas was continued under illumination, and the depth of chlorination was monitored by gas chromatography. After the completion of the reaction, the hydrogen chloride and the excess chlorine gas were driven out by nitrogen gas, and the reaction solution was dedissolved under reduced pressure, and the product chloride was obtained after recovering the carbon tetrachloride. Non-phosgene route N-methylaniline is first reacted with formic acid to form N-methylformylaniline, and then the methyl and aldehyde groups are simultaneously chlorinated in the presence of benzoyl peroxide to obtain the desired chloride. A certain amount of N-methyl aniline and formic acid are added to the reactor, and the reaction liquid is heated to be in a slightly boiling state, Distillate was maintained and distilled out. After about 170 H, the internal temperature of the reaction solution was gradually increased to ° C., and the non-distillate was distilled off. At this time, the reaction was stopped, and the reaction mixture was cooled and distilled under reduced pressure to obtain N-methylformylaniline. Then N-methylformylaniline, carbon tetrachloride and benzoyl perchloride are put into the chlorination reactor, chlorine gas is passed in advance, the temperature is raised to 80 ℃, and the chlorine gas speed is kept at 0.17g/min, gas chromatography tracking analysis and determine the end point of the reaction. After the chlorine gas is stopped, the nitrogen gas is changed to drive through the HCl. After the carbon tetrachloride is recovered, the required chloride is obtained by vacuum distillation and recrystallization. |
