Introduction of a new synthetic route about 13466-35-8

According to the analysis of related databases, 13466-35-8, the application of this compound in the production field has become more and more popular.

Related Products of 13466-35-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, molecular formula is C5H4ClNO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Equipped with a thermometer,Mechanical agitation,Add 150 grams of 1,2-dichloroethane to a 500-mL four-necked flask with a reflux condenser,26.0 g (0.2 mol) of 3-chloro-2-hydroxypyridine (IV) prepared in Example 3,52.0 grams (0.25 moles) of phosphorus pentachloride,Stir the reaction at 60-65 for 10 hours,Then slowly pour the remainder into 200 grams of ice water,Stir well,Then 40wt% sodium hydroxide aqueous solution neutralizes the pH value to 7-8,Layered,Use 1,2-dichloroethane three times for the water layer,50 grams each time,Combine the organic phase,Wash with 30 grams of saturated saline,Then dry with 5 grams of anhydrous sodium sulfate,The solvent was removed by rotary evaporation to obtain 28.1 g of 2,3-dichloropyridine (I), Yield 94.9%, gas phase purity 99.9%.

According to the analysis of related databases, 13466-35-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Zhang Mingfeng; Ju Lizhu; Wang Quanlong; (9 pag.)CN110818621; (2020); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Introduction of a new synthetic route about 13466-35-8

According to the analysis of related databases, 13466-35-8, the application of this compound in the production field has become more and more popular.

Related Products of 13466-35-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, molecular formula is C5H4ClNO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Equipped with a thermometer,Mechanical agitation,Add 150 grams of 1,2-dichloroethane to a 500-mL four-necked flask with a reflux condenser,26.0 g (0.2 mol) of 3-chloro-2-hydroxypyridine (IV) prepared in Example 3,52.0 grams (0.25 moles) of phosphorus pentachloride,Stir the reaction at 60-65 for 10 hours,Then slowly pour the remainder into 200 grams of ice water,Stir well,Then 40wt% sodium hydroxide aqueous solution neutralizes the pH value to 7-8,Layered,Use 1,2-dichloroethane three times for the water layer,50 grams each time,Combine the organic phase,Wash with 30 grams of saturated saline,Then dry with 5 grams of anhydrous sodium sulfate,The solvent was removed by rotary evaporation to obtain 28.1 g of 2,3-dichloropyridine (I), Yield 94.9%, gas phase purity 99.9%.

According to the analysis of related databases, 13466-35-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Zhang Mingfeng; Ju Lizhu; Wang Quanlong; (9 pag.)CN110818621; (2020); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

The important role of 13466-35-8

The chemical industry reduces the impact on the environment during synthesis 13466-35-8, I believe this compound will play a more active role in future production and life.

Related Products of 13466-35-8, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.13466-35-8, name is 3-Chloro-2-hydroxypyridine, molecular formula is C5H4ClNO, molecular weight is 129.54, as common compound, the synthetic route is as follows.

EXAMPLE 1 3-Chloro-5-octyl-2-(4-octyloxyphenyl)pyridine 10.5 ml (203.0 mmol) of bromine are added dropwise at 0 C. to 23.9 g (184.5 mmol) of 3-chloro-2-hydroxypyridine in 240 ml of dimethylformamide, and the mixture is stirred at room temperature for 2 hours. 200 ml of water are subsequently added, and 30 g of sodium sulfite in 100 ml of water are added dropwise. After 15 minutes, the mixture is extracted three times with 200 ml of dichloromethane in each case, the combined organic phases are dried over sodium sulfate and filtered, and the filtrate is evaporated to dryness, giving 36.58 g of 5-bromo-3-chloro-2-hydroxypyridine. STR13 m.p.: 168 C. (decomp.)

The chemical industry reduces the impact on the environment during synthesis 13466-35-8, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Hoechst Aktiengesellschaft; US5629428; (1997); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Extended knowledge of 3-Chloro-2-hydroxypyridine

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Electric Literature of 13466-35-8 , The common heterocyclic compound, 13466-35-8, name is 3-Chloro-2-hydroxypyridine, molecular formula is C5H4ClNO, 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.

To a 500 ml four-necked flask equipped with a thermometer, mechanical stirring, and a reflux condenser was added 150 g of 1,2-dichloroethane, 26.0 g (0.2 mol) of 2-hydroxy-3-chloropyridine prepared in Example 3, 52.0 g (0.25 mole) of phosphorus pentachloride, stir the reaction at 60-65 C for 10 hours, then slowly pour the residue into 200 g of ice water, stir well, and then neutralize the pH value with a 40 wt% sodium hydroxide aqueous solution. 8. The layers were separated. The aqueous layer was 50g with 1,2-dichloroethane three times. The organic phases were combined, washed with 30g of saturated brine, and then dried with 5g of anhydrous sodium sulfate. The solvent was removed by rotary evaporation. 28.1 g of 2,3-dichloropyridine (I) with a yield of 94.9% and a gas phase purity of 99.9%.

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Sun Yulong; Zhang Mingfeng; Chang Renyi; Wang Tao; (10 pag.)CN110818622; (2020); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Sources of common compounds: 3-Chloro-2-hydroxypyridine

The synthetic route of 13466-35-8 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. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, the common compound, a new synthetic route is introduced below. name: 3-Chloro-2-hydroxypyridine

Chlorination: 40 g of 3-chloro-2-hydroxypyridine and 100 g of dichloroethane,DMF0.3g,Phosphorus oxychloride 56g was added to the reaction flask and refluxed.In the control,After the reaction is over,Distilled ethylene dichloride,Slowly add cold water to the reaction solution.After fully hydrolyzing, adjust the pH to 4-5 and steam it.Get 2,3-dichloropyridine,Dry at room temperature and dry at 43gThe purity is 99.1%.

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Kaiyuan People’s Welfare Technology Co., Ltd.; Zhao Fei; Song Liang; Chen Wei; Wei Haihao; Zeng Miao; Xu Jianfeng; (8 pag.)CN107935921; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Sources of common compounds: 3-Chloro-2-hydroxypyridine

The synthetic route of 13466-35-8 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. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, the common compound, a new synthetic route is introduced below. name: 3-Chloro-2-hydroxypyridine

Chlorination: 40 g of 3-chloro-2-hydroxypyridine and 100 g of dichloroethane,DMF0.3g,Phosphorus oxychloride 56g was added to the reaction flask and refluxed.In the control,After the reaction is over,Distilled ethylene dichloride,Slowly add cold water to the reaction solution.After fully hydrolyzing, adjust the pH to 4-5 and steam it.Get 2,3-dichloropyridine,Dry at room temperature and dry at 43gThe purity is 99.1%.

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Kaiyuan People’s Welfare Technology Co., Ltd.; Zhao Fei; Song Liang; Chen Wei; Wei Haihao; Zeng Miao; Xu Jianfeng; (8 pag.)CN107935921; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Sources of common compounds: 3-Chloro-2-hydroxypyridine

The synthetic route of 13466-35-8 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. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, the common compound, a new synthetic route is introduced below. name: 3-Chloro-2-hydroxypyridine

Chlorination: 40 g of 3-chloro-2-hydroxypyridine and 100 g of dichloroethane,DMF0.3g,Phosphorus oxychloride 56g was added to the reaction flask and refluxed.In the control,After the reaction is over,Distilled ethylene dichloride,Slowly add cold water to the reaction solution.After fully hydrolyzing, adjust the pH to 4-5 and steam it.Get 2,3-dichloropyridine,Dry at room temperature and dry at 43gThe purity is 99.1%.

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Kaiyuan People’s Welfare Technology Co., Ltd.; Zhao Fei; Song Liang; Chen Wei; Wei Haihao; Zeng Miao; Xu Jianfeng; (8 pag.)CN107935921; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Brief introduction of 13466-35-8

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 13466-35-8, 3-Chloro-2-hydroxypyridine, other downstream synthetic routes, hurry up and to see.

Electric Literature of 13466-35-8 ,Some common heterocyclic compound, 13466-35-8, molecular formula is C5H4ClNO, 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.

To a stirred solution of triphenylphosphine (814 mg, 3.10 mmol) in THF (7 ml) was added DIAD (603 mul, 3.10 mmol) at 0 oC. The mixture was stirred at 0 oC for about 10 min. To this mixture were added 3-chloro-2-hydroxypyridine (321 mg, 2.481 mmol) and tert- butyl 7-hydroxy-4-azaspiro[2.5]octane-4-carboxylate (470 mg, 2.068 mmol). The mixture was slowly warmed up to RT and stirred at RT overnight. The reaction was quenched with the addition of MeOH (~ 2 ml), and the mixture was concentrated and purified by Isco CombiFlash system on silica gel column (ISCO RediSep gold column, 80g) using 0-100%EtOAc/hexane to give the title compound as an oil after concentration. LCMS m/z [M+H]+ 283.13.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 13466-35-8, 3-Chloro-2-hydroxypyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CLAUSEN, Dane; FRADERA, Xavier; GUO, Liangqin; HAN, Yongxin; HE, Shuwen; HUANG, Xianhai; KOZLOWSKI, Joseph; LI, Guoqing; LIM, Jongwon; MARTINOT, Theodore, A.; PASTERNAK, Alexander; SCIAMMETTA, Nunzio; VERRAS, Andreas; XIAO, Li; YU, Wensheng; ZHANG, Rui; (146 pag.)WO2020/41100; (2020); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

New learning discoveries about 3-Chloro-2-hydroxypyridine

The synthetic route of 13466-35-8 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. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, the common compound, a new synthetic route is introduced below. HPLC of Formula: C5H4ClNO

EXAMPLE 1 3-Chloro-5-octyl-2-(4-octyloxyphenyl)pyridine 10.5 ml (203.0 mmol) of bromine are added dropwise at 0° C. to 23.9 g (184.5 mmol) of 3-chloro-2-hydroxypyridine in 240 ml of dimethylformamide, and the mixture is stirred at room temperature for 2 hours. 200 ml of water are subsequently added, and 30 g of sodium sulfite in 100 ml of water are added dropwise. After 15 minutes, the mixture is extracted three times with 200 ml of dichloromethane in each case, the combined organic phases are dried over sodium sulfate and filtered, and the filtrate is evaporated to dryness, giving 36.58 g of 5-bromo-3-chloro-2-hydroxypyridine. STR13 m.p.: 168° C. (decomp.)

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoechst Aktiengesellschaft; US5629428; (1997); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem