![除草剂噁嗪草酮中间体3,5-二氯苄氯的合成方法](/CN/2018/1/240/images/201811203031.jpg)
基本信息:
- 专利标题: 除草剂噁嗪草酮中间体3,5-二氯苄氯的合成方法
- 专利标题(英):Synthesis method for herbicide oxaziclomefone intermediate 3,5-dichlorobenzyl chloride
- 申请号:CN201811203031.1 申请日:2018-10-16
- 公开(公告)号:CN109232164A 公开(公告)日:2019-01-18
- 发明人: 付洪信 , 杨朝晖 , 王玲
- 申请人: 山东省农药科学研究院 , 济南科海有限公司
- 申请人地址: 山东省济南市北园大街234号
- 专利权人: 山东省农药科学研究院,济南科海有限公司
- 当前专利权人: 山东省农药科学研究院,济南科海有限公司
- 当前专利权人地址: 山东省济南市北园大街234号
- 代理机构: 北京开阳星知识产权代理事务所
- 代理人: 姚金金
- 主分类号: C07C17/00
- IPC分类号: C07C17/00 ; C07C17/16 ; C07C25/02
The invention discloses a synthesis method for herbicide oxaziclomefone intermediate 3,5-dichlorobenzyl chloride, and belongs to the field of pesticide preparation. The synthesis method is characterized in that 3,5-dichlorobenzoic acid, a composite hydrogen compound and metal chloride react under action of polyethylene glycol to obtain 3,5-dichlorobenzyl chloride. A reaction process comprises thefollowing steps: 1) adding 3,5-dichlorobenzoic acid, a solvent A and the composite hydrogen compound into a reaction kettle under a protective gas condition, heating to 40-60 DEG C to react for 5-12 minutes, adding metal chloride, polyethylene glycol and alkaline water, starting ultrasonic assistance, setting power and frequency, controlling the temperature to be 90-110 DEG C, keeping reaction pressure at 1.5-2 barometric pressure, and ending reaction after 2-4 hours; and 2) after the system is cooled, adding a solvent B which is about 1-2 times the volume of reaction liquid, filtering to remove insoluble substances, layering, drying an organic phase with a drying agent, concentrating and re-crystallizing to obtain 3,5-dichlorobenzyl chloride. The synthesis method is fewer in step, less inside reaction, high in yield, less in pollution discharge and safe to operate.