Tag: 92-39-7

A common heterocyclic compound, 92-39-7,2-Chloro-10H-phenothiazine, 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. 92-39-7

(1) Dehydration reaction: 2-chlorophenothiazine, cuprous cyanide, catalyst, quinoline, p-toluenesulfonyl chloride according to moleThe ratio is 1:1.25:0.15:5:0.1 is added to the reactor, and the temperature is raised to 120 C for dehydration reaction, the reaction is 1 hour, and the water is dehydrated to a moisture content of less than 0.1%;The catalyst is a mixture of sodium iodide and lithium iodide, and the molar ratio of sodium iodide to lithium iodide is 1:0.3;(2) Preparation of crude 2-cyanophenothiazine: the temperature of the reactor was raised to 230 C, and the reaction was carried out for 15 hours;(3) Separation of crude 2-cyanophenothiazine: the reactor temperature was lowered to 90 C, and 8 times was added to the reactor.The total amount of moles of the starting material is water, the solid is precipitated and filtered, and the product is extracted with ethyl acetate and concentrated to dryness to give a crude 2-cyanophenothiazine;(4) Purification of 2-cyanophenothiazine: a crude 2-cyanophenothiazine is placed in a mixed solvent of toluene and methanol,The volume ratio of toluene to methanol in the mixed solvent was 1:0.15, the temperature was raised to 120 C for 30 minutes, and the mixture was cooled to 20 C, and the precipitated solid was filtered to obtain 2-cyanophenothiazine.After testing, the yield of 2-cyanophenothiazine prepared in this example was 92.6%, and the purity of the product was 99.61%.The content of the amide was 0.03%.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,92-39-7,2-Chloro-10H-phenothiazine,its application will become more common.

Reference£º
Patent; Ningbo Jinuo Chemicals Co., Ltd.; Peng Zhigang; Yue Mingxin; Qu Qiangzheng; (8 pag.)CN105175355; (2018); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Name is 2-Chloro-10H-phenothiazine, as a common heterocyclic compound, it belongs to thiazines compound, and cas is 92-39-7, its synthesis route is as follows.,92-39-7

(1) Dehydration reaction: 2-chlorophenothiazine, cuprous cyanide, catalyst, quinoline, p-toluenesulfonyl chloride according to moleThe ratio is 1:1.25:0.15:5:0.1 is added to the reactor, and the temperature is raised to 120 C for dehydration reaction, the reaction is 1 hour, and the water is dehydrated to a moisture content of less than 0.1%;The catalyst is a mixture of sodium iodide and lithium iodide, and the molar ratio of sodium iodide to lithium iodide is 1:0.3;(2) Preparation of crude 2-cyanophenothiazine: the temperature of the reactor was raised to 230 C, and the reaction was carried out for 15 hours;(3) Separation of crude 2-cyanophenothiazine: the reactor temperature was lowered to 90 C, and 8 times was added to the reactor.The total amount of moles of the starting material is water, the solid is precipitated and filtered, and the product is extracted with ethyl acetate and concentrated to dryness to give a crude 2-cyanophenothiazine;(4) Purification of 2-cyanophenothiazine: a crude 2-cyanophenothiazine is placed in a mixed solvent of toluene and methanol,The volume ratio of toluene to methanol in the mixed solvent was 1:0.15, the temperature was raised to 120 C for 30 minutes, and the mixture was cooled to 20 C, and the precipitated solid was filtered to obtain 2-cyanophenothiazine.After testing, the yield of 2-cyanophenothiazine prepared in this example was 92.6%, and the purity of the product was 99.61%.The content of the amide was 0.03%.

With the complex challenges of chemical substances, we look forward to future research findings about 2-Chloro-10H-phenothiazine

Reference£º
Patent; Ningbo Jinuo Chemicals Co., Ltd.; Peng Zhigang; Yue Mingxin; Qu Qiangzheng; (8 pag.)CN105175355; (2018); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

The thiazines compound, cas is 92-39-7 name is 2-Chloro-10H-phenothiazine, mainly used in chemical industry, its synthesis route is as follows.

Step: Step 1, the reaction system azeotropic water removal: To the reaction kettle with argon gas was added 50 kg of N-methylpyrrolidone at room temperature, 2-chlorophenothiazine 50 kg, cuprous cyanide 23 kg, lithium iodide 0.23 kg, potassium iodide 3.55 kg and cyclohexane 25 kg, Stirring up to 85C , boiling a total of boiling water, about 40min, measured water 0.04wt.% (Moisture ? 0.05wt.%). Step 2: Preparation of 2-cyanophenothiazine by refluxing reaction: The reaction system after the removal of water continued to warm to 112 C, Atmospheric distillation distillation system in the cyclohexane, cyclohexane can be recycled recycling, Continue to heat up to the reflux state (T = 218 ), insulation reaction 10h, To obtain a reaction product; Step 3, the reaction product after treatment and extraction: After the reaction, the temperature was lowered to 75 C, To the reaction system was added sodium thiosulfate solution (sodium thiosulfate 33 kg and water 250 kg mixed dissolved) Stirring for 2h, cooling to 5 , filtering, the first filter cake and the first filtrate, The first filter cake was dried at 90 C to a moisture content of ? 4 wt.%. The first filter cake was extracted with acetone, The dried cake and acetone 700L, heated to reflux 30min, down to 50 , The second filter cake and the second filtrate were filtered and the second filtrate was concentrated at atmospheric pressure to give 500 L of acetone to give a concentrate, The concentrated liquid for low temperature precipitation, the specific process is to concentrate the solution to 0 , filtration, Dried 2-cyanophenothiazine crude 45kg, 98% purity, amide impurity 0.9%.Step 4: Purification of crude 2-cyanophenothiazine: 2-cyanophenothiazine crude 45kg and acetone 36kg heated to reflux, reflux insulation 30min. Cooled to 0 C, filtered and dried to give 4-cyano phenothiazine 43.2 kg, purity ?99% Amide impurities ? 0.1%, yield: 90.0%This example gives an industrial preparation method of an environment-friendly 2-cyanophenothiazine, The method of other processes and implementation Example 1 is the same, the difference is only: In the third step, the mass of the dried first filter cake and the ratio of the second organic solvent acetone used in the first filter cake Was adjusted to 1:15 from 1: 8 of Example 1. The yield of 2-cyanophenothiazine was 90.2% based on 2-chlorophenothiazine

With the rapid development of chemical substances, we look forward to future research findings about 92-39-7

Reference£º
Patent; Xi’an Caijing Optoelectric Technology Co., Ltd.; Gao Aiai; Zhao Qunxing; Zhou Bugao; Fan Jia; Bie Guojun; Yan Xiaoliang; Lan Aihu; Guo Chuang; Li Jian; Xu Lei; Zhang Weijie; Wang Li; (11 pag.)CN106946811; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.92-39-7,2-Chloro-10H-phenothiazine,as a common compound, the synthetic route is as follows.

(1) Dehydration reaction: 2-chlorophenothiazine, cuprous cyanide, catalyst, quinoline, p-toluenesulfonyl chloride according to moleThe ratio is 1:1.25:0.15:5:0.1 is added to the reactor, and the temperature is raised to 120 C for dehydration reaction, the reaction is 1 hour, and the water is dehydrated to a moisture content of less than 0.1%;The catalyst is a mixture of sodium iodide and lithium iodide, and the molar ratio of sodium iodide to lithium iodide is 1:0.3;(2) Preparation of crude 2-cyanophenothiazine: the temperature of the reactor was raised to 230 C, and the reaction was carried out for 15 hours;(3) Separation of crude 2-cyanophenothiazine: the reactor temperature was lowered to 90 C, and 8 times was added to the reactor.The total amount of moles of the starting material is water, the solid is precipitated and filtered, and the product is extracted with ethyl acetate and concentrated to dryness to give a crude 2-cyanophenothiazine;(4) Purification of 2-cyanophenothiazine: a crude 2-cyanophenothiazine is placed in a mixed solvent of toluene and methanol,The volume ratio of toluene to methanol in the mixed solvent was 1:0.15, the temperature was raised to 120 C for 30 minutes, and the mixture was cooled to 20 C, and the precipitated solid was filtered to obtain 2-cyanophenothiazine.After testing, the yield of 2-cyanophenothiazine prepared in this example was 92.6%, and the purity of the product was 99.61%.The content of the amide was 0.03%.

#N/A

Reference£º
Patent; Ningbo Jinuo Chemicals Co., Ltd.; Peng Zhigang; Yue Mingxin; Qu Qiangzheng; (8 pag.)CN105175355; (2018); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

92-39-7, 2-Chloro-10H-phenothiazine is a thiazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step: Step 1, the reaction system azeotropic water removal: To the reaction kettle with argon gas was added 50 kg of N-methylpyrrolidone at room temperature, 2-chlorophenothiazine 50 kg, cuprous cyanide 23 kg, lithium iodide 0.23 kg, potassium iodide 3.55 kg and cyclohexane 25 kg, Stirring up to 85C , boiling a total of boiling water, about 40min, measured water 0.04wt.% (Moisture ? 0.05wt.%). Step 2: Preparation of 2-cyanophenothiazine by refluxing reaction: The reaction system after the removal of water continued to warm to 112 C, Atmospheric distillation distillation system in the cyclohexane, cyclohexane can be recycled recycling, Continue to heat up to the reflux state (T = 218 ), insulation reaction 10h, To obtain a reaction product; Step 3, the reaction product after treatment and extraction: After the reaction, the temperature was lowered to 75 C, To the reaction system was added sodium thiosulfate solution (sodium thiosulfate 33 kg and water 250 kg mixed dissolved) Stirring for 2h, cooling to 5 , filtering, the first filter cake and the first filtrate, The first filter cake was dried at 90 C to a moisture content of ? 4 wt.%. The first filter cake was extracted with acetone, The dried cake and acetone 700L, heated to reflux 30min, down to 50 , The second filter cake and the second filtrate were filtered and the second filtrate was concentrated at atmospheric pressure to give 500 L of acetone to give a concentrate, The concentrated liquid for low temperature precipitation, the specific process is to concentrate the solution to 0 , filtration, Dried 2-cyanophenothiazine crude 45kg, 98% purity, amide impurity 0.9%.Step 4: Purification of crude 2-cyanophenothiazine: 2-cyanophenothiazine crude 45kg and acetone 36kg heated to reflux, reflux insulation 30min. Cooled to 0 C, filtered and dried to give 4-cyano phenothiazine 43.2 kg, purity ?99% Amide impurities ? 0.1%, yield: 90.0%This example gives an industrial preparation method of an environment-friendly 2-cyanophenothiazine, The method of other processes and implementation Example 1 is the same, the difference is only: In the third step, the mass of the dried first filter cake and the ratio of the second organic solvent acetone used in the first filter cake Was adjusted to 1:15 from 1: 8 of Example 1. The yield of 2-cyanophenothiazine was 90.2% based on 2-chlorophenothiazine

The synthetic route of 92-39-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Xi’an Caijing Optoelectric Technology Co., Ltd.; Gao Aiai; Zhao Qunxing; Zhou Bugao; Fan Jia; Bie Guojun; Yan Xiaoliang; Lan Aihu; Guo Chuang; Li Jian; Xu Lei; Zhang Weijie; Wang Li; (11 pag.)CN106946811; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem