
基本信息:
- 专利标题: 一种苯丙烯氟菌唑中间体3-(二氟甲基)-1-甲基-1H-吡唑-4-羧酸的合成方法
- 专利标题(英):Synthesis method for allylbenzene triflumizole intermediate 3-(difluoromethyl)-1-metyl-1H-pyrazol-4-carboxylic acid
- 申请号:CN201811203028.X 申请日:2018-10-16
- 公开(公告)号:CN109232425A 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: C07D231/14
- IPC分类号: C07D231/14
The invention discloses a synthesis method for allylbenzene triflumizole intermediate 3-(difluoromethyl)-1-metyl-1H-pyrazol-4-carboxylic acid, and belongs to the field of pesticide pharmacy. The synthesis method is characterized in that 3-(difluoromethyl)-1-metyl-1H-pyrazol-4-carboxylic acid is obtained by reacting 3-difluoromethyl-1-methyl-1H-pyrazol and chloro-formate under the action of a catalyst, and a reaction process comprises the following steps: 1) uniformly mixing 3-difluoromethyl-1-methyl-1H-pyrazol, the catalyst and a solvent A, introducing protective gas, controlling pressure to 10-15 barometric pressures, controlling the temperature to 80-110 DEG C, adding chloro-formate, and controlling adding time of chloro-formate to be 40-60 minutes; increasing the reaction temperature to130-150 DEG C after adding is completed, slowly controlling to reduce pressure to 7-9 barometric pressures within 60-90 minutes, and continuously reacting for 40-62 hours; 2) cooling a system, filtering to remove solid, adding filtrate into water with the volume being 6-10 times of that of the filtrate, regulating pH to 2-3 with acid, extracting with a solvent B, washing extracting liquor with water, drying with a drying agent, and concentrating to obtain a product. The synthesis method has the advantages of relatively short steps and relatively low process cost.
IPC结构图谱:
C | 化学;冶金 |
--C07 | 有机化学 |
----C07D | 杂环化合物 |
------C07D231/00 | 杂环化合物,含1,2-二唑或氢化1,2-二唑环 |
--------C07D231/02 | .不与其他环稠合 |
----------C07D231/06 | ..环原子间或环原子与非环原子间有1个双键 |
------------C07D231/14 | ...有杂原子或有以3个键连杂原子、其中最多以1个键连卤素的碳原子,例如,酯基或腈基,直接与环碳原子相连 |