Some scientific research about 3,4-Dichlorobenzonitrile

According to the analysis of related databases, 6574-99-8, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 6574-99-8 as follows. SDS of cas: 6574-99-8

The solvent and catalyst recovered in Example 2 were used for feeding.1) In the reaction kettle with a reflux water separation device, add the anhydrous aprotic polar solvent 1,3-dimethylimidazoline used in Example 2 and make up 2000 kg with a new solvent.Raw materials 3,4-dichlorobenzonitrile 1000 kg, water agent 200 kg toluene, heated to 90 ~ 120 reflux, water separation for 1 to 2 hours, until the water in the kettle <0.05% 2) Add 800 kg of potassium fluoride and 45 kg of catalyst to the reaction kettle, raise the temperature to 130 150 , and reflux for 2 to 3 hours; 3) Turn on the vacuum pump, the vacuum degree is -0.1MPa, the top temperature of the reaction kettle tower is 90-115 C, and the toluene is collected, and the fractions are collected; 4) Continue to increase the temperature. When the temperature in the reactor reaches 190 200 and the top temperature reaches 170-180 , the crude 3,4-difluorobenzonitrile will be collected. When the content of 3,4-difluorobenzonitrile in the reactor is at At 89.0-89.5%, the reaction is deemed complete and the crude product is 818 kg; 5) Turn off the hot oil pump, turn on the cold oil system, the temperature in the reaction kettle drops below 100 C, put the materials in the reaction kettle into a centrifuge, the filtrate is pumped into the reaction kettle for the next feeding, and the solid materials are bagged; 6) The crude product 3,4-difluorobenzonitrile is drawn into the rectification kettle, stirring is started, and the fractions of 179-181 C are collected at elevated temperature and pressure to obtain the finished product 3,4-difluorobenzonitrile 743 kg, content 99.63%, yield 93.0%; after distillation, the residual liquid is sent to the reactor for the next feeding. According to the analysis of related databases, 6574-99-8, the application of this compound in the production field has become more and more popular. Reference:
Patent; Ji’ning Kangsheng Rainbow Biological Technology Co., Ltd.; Qian Jidong; Huang Dingqian; Sheng Rui; Yan Weiwei; (8 pag.)CN110804001; (2020); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Continuously updated synthesis method about 6574-99-8

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,4-Dichlorobenzonitrile, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 6574-99-8, name is 3,4-Dichlorobenzonitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 6574-99-8, Application In Synthesis of 3,4-Dichlorobenzonitrile

The solvent and catalyst recovered in Example 2 were used for feeding.1) In the reaction kettle with a reflux water separation device, add the anhydrous aprotic polar solvent 1,3-dimethylimidazoline used in Example 2 and make up 2000 kg with a new solvent.Raw materials 3,4-dichlorobenzonitrile 1000 kg, water agent 200 kg toluene, heated to 90 ~ 120 reflux, water separation for 1 to 2 hours, until the water in the kettle <0.05% 2) Add 800 kg of potassium fluoride and 45 kg of catalyst to the reaction kettle, raise the temperature to 130 150 , and reflux for 2 to 3 hours; 3) Turn on the vacuum pump, the vacuum degree is -0.1MPa, the top temperature of the reaction kettle tower is 90-115 C, and the toluene is collected, and the fractions are collected; 4) Continue to increase the temperature. When the temperature in the reactor reaches 190 200 and the top temperature reaches 170-180 , the crude 3,4-difluorobenzonitrile will be collected. When the content of 3,4-difluorobenzonitrile in the reactor is at At 89.0-89.5%, the reaction is deemed complete and the crude product is 818 kg; 5) Turn off the hot oil pump, turn on the cold oil system, the temperature in the reaction kettle drops below 100 C, put the materials in the reaction kettle into a centrifuge, the filtrate is pumped into the reaction kettle for the next feeding, and the solid materials are bagged; 6) The crude product 3,4-difluorobenzonitrile is drawn into the rectification kettle, stirring is started, and the fractions of 179-181 C are collected at elevated temperature and pressure to obtain the finished product 3,4-difluorobenzonitrile 743 kg, content 99.63%, yield 93.0%; after distillation, the residual liquid is sent to the reactor for the next feeding. At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,4-Dichlorobenzonitrile, and friends who are interested can also refer to it. Reference:
Patent; Ji’ning Kangsheng Rainbow Biological Technology Co., Ltd.; Qian Jidong; Huang Dingqian; Sheng Rui; Yan Weiwei; (8 pag.)CN110804001; (2020); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Extended knowledge of 6574-99-8

Statistics shows that 3,4-Dichlorobenzonitrile is playing an increasingly important role. we look forward to future research findings about 6574-99-8.

Reference of 6574-99-8, These common heterocyclic compound, 6574-99-8, name is 3,4-Dichlorobenzonitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: Hydrogen chloride gas was passed through a solution of 4-chlorobenzonitrile (9b, 25.0 g) in chloroform (350 mL) and ethanol (100 mL) at -78 C for 0.5 h. Then the solution was warmed up to room temperature, and stirred at room temperature overnight. The solution was evaporated in vacuo, and the resulting residue was dissolved with ethanol (500 mL). To the solution was added ammonium carbonate (90.0 g), and the reaction mixture was stirred at room temperature for 3 days. To the mixture was added water (300 mL), and ethanol was removed by concentration in vacuo. The resulting solid was collected by filtration, washed with water and dried in vacuo to give 12b (25.4 g, 71%) as a white solid.

Statistics shows that 3,4-Dichlorobenzonitrile is playing an increasingly important role. we look forward to future research findings about 6574-99-8.

Reference:
Article; Negoro, Kenji; Yonetoku, Yasuhiro; Misawa-Mukai, Hana; Hamaguchi, Wataru; Maruyama, Tatsuya; Yoshida, Shigeru; Takeuchi, Makoto; Ohta, Mitsuaki; Bioorganic and Medicinal Chemistry; vol. 20; 17; (2012); p. 5235 – 5246;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

New learning discoveries about 6574-99-8

The synthetic route of 6574-99-8 has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6574-99-8, name is 3,4-Dichlorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H3Cl2N

To the reaction vessel of the dry strip rectification column, 350 g of N-methylpyrrolidone (NMP) and anhydrous potassium fluoride (230 g, 3.96 mol) were placed.Add 150g of toluene and reflux to separate water for about 2 hours. After the end of water separation, the toluene is distilled out and recycled for the next application., 3,4-dichlorobenzonitrile (200 g, 1.16 mol), bis-(N,N’-1,3-dimethyl-2-imidazolidinyl)-ammonium chloride (10 g, 0.04 mol) ),Sodium lauryl sulfate (5 g) and sodium thiosulfate (10 g) were heated to 200-210 C for 4 hours.The rectification column received 157 g of a crude product of 3,4-difluorobenzonitrile, and the crude product was subjected to secondary rectification to obtain 146 g of a 3,4-difluorobenzonitrile product having a purity of 99% and a molar yield of 90.7%..

The synthetic route of 6574-99-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Feng Shan Group Co., Ltd.; Chen Baoming; Wang Jinyang; Zhang Qingbao; Ma Tiantian; Dou Feiyang; Yao Jinli; Li Xing; Li Junqing; Wang Bo; Shan Yongxiang; Yin Ping; Yin Fengshan; (8 pag.)CN108409605; (2018); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Introduction of a new synthetic route about 6574-99-8

The synthetic route of 3,4-Dichlorobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference of 6574-99-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6574-99-8, name is 3,4-Dichlorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General Procedure C. The nitrile (10 mmol) was added in several portions, over 0.5 h to a solution of the nBuMgCl (12 mmol) in toluene (20 mL). The reactions were monitored by TLC and heated where necessary. Generally, after 2 h stirring at room temperature, the reaction was complete. The reaction mixture was poured onto ice and concentrated H2S04 (2 mL) was added. Hydrolysis of the intermediate imine usually occurred at room temperature after several minutes, however, for some substrates, heating was necessary to effect this transformation. The organics were extracted into Et20, dried (MgS04), filtered, and reduced to an oil in vacuo. Example 58 1-(3, 4-Dichloro-phenyl)-pentan-l-one. Following General Procedure C, this compound was prepared in 93% yield and employed in the next step of the reaction as the crude material.

The synthetic route of 3,4-Dichlorobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PRESIDENT AND FELLOWS OF HARVARD COLLEGE; ORGANIX, INC.; WO2005/34878; (2005); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts