Category: 5203-77-0

Electric Literature of 5203-77-0, 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. 5203-77-0 name is 1,3-Dimethyl-1H-pyrazol-5-ol, This 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.

General procedure: To a flame-dried Schlenk tube was added electron-rich aromatic (0.5mmol), CF3SO2Na (118mg, 0.7mmol) dry 1,4-dioxane or CH3CN (1mL). The mixture was heated to 60C by a preheated oil bath. PhPCl2 (125mg, 0.7 mmoL) was added. The reaction mixture was stirred at 70C for the indicated time. Then the reaction mixture was cooled to room temperature. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography to afford the pure product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Dimethyl-1H-pyrazol-5-ol, and friends who are interested can also refer to it.

Reference:
Article; Zhao, Xia; Zheng, Xiancai; Tian, Miaomiao; Sheng, Jianqiao; Tong, Yifan; Lu, Kui; Tetrahedron; vol. 73; 51; (2017); p. 7233 – 7238;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Application of 5203-77-0, A common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, molecular formula is C5H8N2O, 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.

Intermediate 9 (4 mmol), dissolved in dry dichloromethane( 60 mL), and DCC (4.8 mmol) were mixed together and stirred at room temperature for 1 h. Then 1,3-dimethyl-1H-pyrazol-5-ol (4 mmol) and DMAP (0.4 mmol) were added to the above solution,and stirred for a further 24-36 h at room temperature. After adding dichloromethane (30 mL), the resultant mixture was washed sequentially with 2 N hydrochloric acid (100 mL), saturated NaHCO3 and saturated brine and dried over anhydrous sodium sulfate.The residue solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V/V = 1/2) to obtain the desired intermediate 10.

The synthetic route of 5203-77-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xu, Yu-Ling; Lin, Hong-Yan; Cao, Run-Jie; Ming, Ze-Zhong; Yang, Wen-Chao; Yang, Guang-Fu; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5194 – 5211;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference of 5203-77-0, These common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, 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.

Weigh 4.0g (0.036mol) 1,3- dimethyl-5-pyrazolone-ol in 250mLthree-necked flask was added 50mL1,2-Dichloroethane was dissolved, weighing 12g (0.12mol) oftriethylamine in the system. Under ice cooling, the mixture of intermediate(b-2)The reaction solution (0.030mol press note) was addeddropwise to the system, a solution process using argon. After the reaction 1hHPLC trace transShall, after completion of the reaction raw reaction solutioncontaining the intermediate (b-3) a. To the reaction solution containingintermediate (b-3) in additional3.0g (0.030mol) of triethylamine and 0.5mL acetonecyanohydrin, temperature control and the use of argon, the reaction 2h at 50 ~60 ,The reaction was followed by HPLC. After completion of thereaction was added 100mL of water was slowly added dropwise HCl, stirring atroom temperature, until pH = 3 or so. ExtractionThe aqueous layer was removed, and the organic layer waswashed twice with 200mL of water, dried over anhydrous sodium sulfate, theorganic solvent was removed by rotary evaporation to afford 8.1gA tan solid, a powdered compound b.

The synthetic route of 5203-77-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lian, Lei; Zheng, Yurong; He, Bin; Pengxue, Gang; Jin, Tao; Cui, Qi; (63 pag.)CN105503728; (2016); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Related Products of 5203-77-0, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, This compound has unique chemical properties. The synthetic route is as follows.

At room temperature, 1,3-dimethyl-1hydro-pyrazole-5-ol (0.65 g, 0.0058 mol) and (0.48 g, 0.012 mol) sodium hydroxide were sequentially dissolved in 20 ml of dichloromethane.The low temperature bath was cooled to -4 C. To the above mixture was added dropwise 3,7-dichloro-5-(methylsulfonyl)-6-(((tetrahydrofuran-3-yl)methoxy)methyl)quinoline-8-carbonyl chloride (3.81 g, 0.0084 mol),The dropping rate was 4 drops / 30 seconds. After the addition was complete, the mixture naturally rose to room temperature and reacted for 5 hours.To the reaction mixture was added 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and dichloromethane (3 * 15 ml) was extracted. The organic layers were combined, washed with water (1 * 15 ml), washed with saturated brine, and dried over anhydrous magnesium sulfate.The product was dissolved under reduced pressure to obtain 2.12 g of the product with a yield of 70%

The chemical industry reduces the impact on the environment during synthesis 1,3-Dimethyl-1H-pyrazol-5-ol. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Shandong Joint Pesticide Co., Ltd.; Tang Jianfeng; Chi Huiwei; Wu Jianting; Yuan Xue; Liu Ying; (52 pag.)CN110615781; (2019); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, belongs to pyrazoles-derivatives 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 5203-77-0, Recommanded Product: 1,3-Dimethyl-1H-pyrazol-5-ol

Step 7: Synthesis of 1,3-dimethyl-5-(2-methyl-3-(methylthio)-4-(pentafluoroethyl)benzoyloxy)pyrazole360 mg (1.20 mmol) of 2-methyl-3-(methylthio)-4-(pentafluoroethyl)benzoic acid were introduced into 20 ml of dry dichloromethane and admixed in succession with 198 mg (1.56 mmol) of oxalyl dichloride and also with two drops of N,N-dimethyl-formamide. After the end of evolution of gas, the mixture was heated under reflux for 10 minutes. When a check on the reaction by thin-layer chromatography had indicated complete conversion, the contents were freed from the solvent, and the residue was then taken up in 20 ml of dry dichloromethane. The mixture was admixed with 161 mg (1.44 mmol) of 5-hydroxy-1,3-dimethylpyrazole, and then 243 mg (2.40 mmol) of triethylamine were added dropwise. The contents were stirred at RT for 16 hours. For working up, 3 ml of 1M hydrochloric acid were added, and, following phase separation, the organic phase was freed from the solvent. The residue, finally, was purified by chromatography, giving 410 mg of clean product.

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, 1,3-Dimethyl-1H-pyrazol-5-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER CROPSCIENCE AG; US2012/21903; (2012); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, belongs to pyrazoles-derivatives 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 5203-77-0, SDS of cas: 5203-77-0

Intermediate 9 (4 mmol), dissolved in dry dichloromethane( 60 mL), and DCC (4.8 mmol) were mixed together and stirred at room temperature for 1 h. Then 1,3-dimethyl-1H-pyrazol-5-ol (4 mmol) and DMAP (0.4 mmol) were added to the above solution,and stirred for a further 24-36 h at room temperature. After adding dichloromethane (30 mL), the resultant mixture was washed sequentially with 2 N hydrochloric acid (100 mL), saturated NaHCO3 and saturated brine and dried over anhydrous sodium sulfate.The residue solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V/V = 1/2) to obtain the desired intermediate 10.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Dimethyl-1H-pyrazol-5-ol, and friends who are interested can also refer to it.

Reference:
Article; Xu, Yu-Ling; Lin, Hong-Yan; Cao, Run-Jie; Ming, Ze-Zhong; Yang, Wen-Chao; Yang, Guang-Fu; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5194 – 5211;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, molecular formula is C5H8N2O, 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. Safety of 1,3-Dimethyl-1H-pyrazol-5-ol

Intermediate 9 (4 mmol), dissolved in dry dichloromethane( 60 mL), and DCC (4.8 mmol) were mixed together and stirred at room temperature for 1 h. Then 1,3-dimethyl-1H-pyrazol-5-ol (4 mmol) and DMAP (0.4 mmol) were added to the above solution,and stirred for a further 24-36 h at room temperature. After adding dichloromethane (30 mL), the resultant mixture was washed sequentially with 2 N hydrochloric acid (100 mL), saturated NaHCO3 and saturated brine and dried over anhydrous sodium sulfate.The residue solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V/V = 1/2) to obtain the desired intermediate 10.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5203-77-0, its application will become more common.

Reference:
Article; Xu, Yu-Ling; Lin, Hong-Yan; Cao, Run-Jie; Ming, Ze-Zhong; Yang, Wen-Chao; Yang, Guang-Fu; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5194 – 5211;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, molecular formula is C5H8N2O, 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. Quality Control of 1,3-Dimethyl-1H-pyrazol-5-ol

General procedure: Intermediate 7 (4mmol), dissolved in dry dichloromethane (60mL), and PCl5 (4.2mmol) were added and stirred at room temperature for 1h. The solvent was moved out under reduced pressure to afford acid chloride, the acid chloride was then dissolved in dry CH2Cl2 (60mL), Then 1-methyl-1H-pyrazol-5-ol (4mmol) and Et3N (4.8mmol) were added to the above solution, and stirred for a further 18-24hat room temperature. After adding dichloromethane (30mL), the resultant mixture was washed sequentially with 2N hydrochloric acid (100mL), saturated NaHCO3 and saturated NaCl and dried over Na2SO4. The rest of the solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V:V = 1:2) to obtain the desired intermediate 8 as a write powder (30%-70%). 4.1.10 1-methyl-1H-pyrazol-5-yl3-methyl-2-oxo-1-propyl-2,3-dihydro-1H-benzo[d] imidazole- 5-carboxylate Yield: 45%. m.p. 107-108C. 1H NMR (600MHz, CDCl3) delta 8.01 (dd, J=8.4, 1.2Hz, 1H), 7.77 (d, J=1.2Hz, 1H), 7.48 (d, J=1.8Hz, 1H), 7.10 (d, J=8.4Hz, 1H), 6.20 (d, J=1.8Hz, 1H), 3.92 (t, J=7.2Hz, 2H), 3.80 (s, 3H), 3.51 (s, 3H), 1.91-1.71 (m, 2H), 1.00 (t, J=7.8Hz, 3H). EI-MS (m/z): 314.18 (M)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5203-77-0, its application will become more common.

Reference:
Article; Xu, Yu-Ling; Lin, Hong-Yan; Ruan, Xu; Yang, Sheng-Gang; Hao, Ge-Fei; Yang, Wen-Chao; Yang, Guang-Fu; European Journal of Medicinal Chemistry; vol. 92; (2015); p. 427 – 438;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

General procedure: Intermediate 7 (4mmol), dissolved in dry dichloromethane (60mL), and PCl5 (4.2mmol) were added and stirred at room temperature for 1h. The solvent was moved out under reduced pressure to afford acid chloride, the acid chloride was then dissolved in dry CH2Cl2 (60mL), Then 1-methyl-1H-pyrazol-5-ol (4mmol) and Et3N (4.8mmol) were added to the above solution, and stirred for a further 18-24hat room temperature. After adding dichloromethane (30mL), the resultant mixture was washed sequentially with 2N hydrochloric acid (100mL), saturated NaHCO3 and saturated NaCl and dried over Na2SO4. The rest of the solution was evaporated in vacuum and purified by silica gel column chromatography using gradient elution of ethyl acetate/hexane (V:V = 1:2) to obtain the desired intermediate 8 as a write powder (30%-70%). 4.1.10 1-methyl-1H-pyrazol-5-yl3-methyl-2-oxo-1-propyl-2,3-dihydro-1H-benzo[d] imidazole- 5-carboxylate Yield: 45%. m.p. 107-108C. 1H NMR (600MHz, CDCl3) delta 8.01 (dd, J=8.4, 1.2Hz, 1H), 7.77 (d, J=1.2Hz, 1H), 7.48 (d, J=1.8Hz, 1H), 7.10 (d, J=8.4Hz, 1H), 6.20 (d, J=1.8Hz, 1H), 3.92 (t, J=7.2Hz, 2H), 3.80 (s, 3H), 3.51 (s, 3H), 1.91-1.71 (m, 2H), 1.00 (t, J=7.8Hz, 3H). EI-MS (m/z): 314.18 (M)+.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Xu, Yu-Ling; Lin, Hong-Yan; Ruan, Xu; Yang, Sheng-Gang; Hao, Ge-Fei; Yang, Wen-Chao; Yang, Guang-Fu; European Journal of Medicinal Chemistry; vol. 92; (2015); p. 427 – 438;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Electric Literature of 5203-77-0, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, This compound has unique chemical properties. The synthetic route is as follows.

At room temperature, 1,3-dimethyl-1H-pyrazole-5-ol (1.12 g, 0.01 mol) and (2.02 g, 0.02 mol) triethylamine were sequentially dissolved in 20 ml of dichloromethane.The low temperature bath was cooled to 3 C. To the above mixture, 5-(methylsulfonyl)quinoline-8-carbonyl chloride (2.83 g, 0.0105 mol) was added dropwise at a drop rate of 1 drop / 30 seconds. After the dropwise addition, the mixture naturally rose to room temperature and reacted for 5 hours. .To the reaction mixture was added 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with dichloromethane (3 * 15 ml). The organic layers were combined, Wash with water (1 * 15ml), saturated brine, and dry over anhydrous magnesium sulfate.The product was desolvated under reduced pressure to obtain 2.76 g of the product with a yield of 80%

The chemical industry reduces the impact on the environment during synthesis 1,3-Dimethyl-1H-pyrazol-5-ol. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Shandong Joint Pesticide Co., Ltd.; Tang Jianfeng; Chi Huiwei; Wu Jianting; Yuan Xue; Liu Ying; (52 pag.)CN110615781; (2019); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics