阅读说明：本技术 一种合成腐霉利的方法 (Method for synthesizing procymidone ) 是由 柴明根 高金平 廖永 张东辉 于 2020-07-27 设计创作，主要内容包括：本发明公开了一种合成腐霉利的方法,该合成腐霉利的方法具体步骤如下：S1：向500ml带有搅拌的四口烧瓶中投入甲基氯丙酸甲酯、氨水和催化剂,混合搅拌,备用；S2：进行升温回流反应,反应时间为4h,中间过程控制甲基氯丙酸甲酯<1％；S3：温度升温至60℃时,加入水,1,3,5-均三氯苯,进行升温回流反应,中间过程控制1,3,5-均三氯苯含量<0.5％,温度至60℃,进行放料,获得固体物备用；S4：对放料后获得的固体物进行水洗两次,再进行酒精清洗1次,备用；S5：对经过2次水洗,1次酒精清洗的物质进行烘干,获得腐霉利。本发明路线,没有选用高价原料3,5-二氯苯胺,具有三废少,产品收率高,质量好的特点,具有明显的经济和社会效益。(The invention discloses a method for synthesizing procymidone, which comprises the following specific steps: s1: adding methyl chloropropionate, ammonia water and a catalyst into a 500ml four-neck flask with a stirrer, and mixing and stirring for later use; s2: heating and refluxing for 4h, and controlling methyl chloropropionate to be less than 1% in the intermediate process; s3: when the temperature is raised to 60 ℃, adding water and 1,3, 5-sym-trichlorobenzene, carrying out heating reflux reaction, controlling the content of the 1,3, 5-sym-trichlorobenzene to be less than 0.5% in the middle process, and discharging when the temperature is raised to 60 ℃ to obtain a solid for later use; s4: washing the solid obtained after discharging twice with water, and then washing with alcohol for 1 time for later use; s5: and (3) drying the substance washed by the water for 2 times and the alcohol for 1 time to obtain the procymidone. The route of the invention does not select high-price raw material 3, 5-dichloroaniline, has the characteristics of less three wastes, high product yield and good quality, and has obvious economic and social benefits.)

1. A method for synthesizing procymidone, which is characterized by comprising the following steps: the method for synthesizing the procymidone comprises the following specific steps:

s1: adding methyl chloropropionate, ammonia water and a catalyst into a 500ml four-neck flask with a stirrer, and mixing and stirring for later use;

s2: heating and refluxing for 4h, and controlling methyl chloropropionate to be less than 1% in the intermediate process;

s3: when the temperature is raised to 60 ℃, adding water and 1,3, 5-sym-trichlorobenzene, carrying out heating reflux reaction, controlling the content of the 1,3, 5-sym-trichlorobenzene to be less than 0.5% in the middle process, and discharging when the temperature is raised to 60 ℃ to obtain a solid for later use;

s4: washing the solid obtained after discharging twice with water, and then washing with alcohol for 1 time for later use;

s5: and (3) drying the substance washed by the water for 2 times and the alcohol for 1 time to obtain the procymidone.

2. A method of synthesizing procymidone according to claim 1, wherein: the molar ratio of methyl methacrylate to ammonia water was: 1:1.1-1.5.

3. A method of synthesizing procymidone according to claim 1, wherein: the catalyst is an organometallic complex of copper or antimony.

4. A method of synthesizing procymidone according to claim 1, wherein: the molar ratio of methyl chloropropionate to 1,3, 5-sym-trichlorobenzene is 1.1-1.3: 1.

5. A method of synthesizing procymidone according to claim 1, wherein: the 1,3, 5-trichlorobenzene may be replaced by 1, 3-dichloro-5-bromobenzene.

Technical Field

The invention relates to the technical field of procymidone, in particular to a method for synthesizing procymidone.

Background

Procymidone is a systemic fungicide developed and produced by Sumitomo chemical industry Co. Can effectively inhibit the synthesis of triglyceride in the thalli, and has double functions of protection and treatment. Mainly acts on cell membranes, hinders the synthesis of normal cell walls at the top of hyphae, and inhibits the development of hyphae. The main control objects are sclerotinia sclerotiorum and gray mold, and the composition has good protection effect, long lasting period and can prevent the development of scabs. Is suitable for fruit trees such as corn, cucumber, tomato, scallion, rape, grape, strawberry, peach, cherry, etc. The main preparation types are: 50% of procymidone wettable powder, 30% of granular fumigant, 25% of flowable powder and colloidal suspension. According to data query, the technology for synthesizing procymidone mainly comprises the following steps: and (3) reacting methyl methacrylate with 3, 5-dichloroaniline to obtain the procymidone.

The 3, 5-dichloroaniline used as the raw material in the process is difficult to source and expensive, and a large amount of acidic wastewater and waste residues are generated during the production of the raw material; at present, the domestic procymidone is synthesized by adopting the process, and a plurality of environmental pollution factors and cost pressure exist.

Disclosure of Invention

The invention aims to provide a method for synthesizing procymidone, which comprises the following specific steps:

s1: adding methyl chloropropionate, ammonia water and a catalyst into a 500ml four-neck flask with a stirrer, and mixing and stirring for later use;

s2: heating and refluxing for 4h, and controlling methyl chloropropionate to be less than 1% in the intermediate process;

s3: when the temperature is raised to 60 ℃, adding water and 1,3, 5-sym-trichlorobenzene, carrying out heating reflux reaction, controlling the content of the 1,3, 5-sym-trichlorobenzene to be less than 0.5% in the middle process, and discharging when the temperature is raised to 60 ℃ to obtain a solid for later use;

s4: washing the solid obtained after discharging twice with water, and then washing with alcohol for 1 time for later use;

s5: and (3) drying the substance washed by the water for 2 times and the alcohol for 1 time to obtain the procymidone.

Preferably, the molar ratio of methyl methacrylate to ammonia is: 1:1.1-1.5.

Preferably, the catalyst is an organometallic complex of copper or antimony.

Preferably, the molar ratio of the methyl chloropropionate to the 1,3, 5-trichlorobenzene is 1.1-1.3: 1.

Preferably, the 1,3, 5-trichlorobenzene can be replaced by 1, 3-dichloro-5-bromobenzene.

Compared with the prior art, the invention has the beneficial effects that: the route of the invention does not select high-price raw material 3, 5-dichloroaniline, has the characteristics of less three wastes, high product yield and good quality, and has obvious economic and social benefits.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.