Category: 694-48-4

Application of 694-48-4,Some common heterocyclic compound, 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, molecular formula is C5H8N2, 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.

In a 5 L reactor, equipped with a stirrer, a reflux condenser, an argon inlet, thermometer and dropping funnel, 1,3-dimethyl-1H-pyrazole(500 g, 5.2 mol) was added slowly with stirring to acetic anhydride (1950 mL, 2125 g, 20.8 mol), while maintaining the temperature below 45 C. Concd H2SO4(50 mL, 92 g, 0.94 mol) was added with cooling and stirring and the mixture then was gradually heated to reflux and held at reflux for 6 h. The mixture was then cooled, evaporated at 70 C/7 Torr, and treated with crushed ice (2 kg). By carefully addition of 40% NaOH solution, the pH of the reaction mixture was adjusted to pH 8, then the organic phase was separated and the aqueous phase was extracted with CH2Cl2(2 × 1000 mL).The combined organic phases were washed successively with H2O(500 mL) and brine (500 mL), and dried over MgSO4. The solvent was removed at 7 Torr, and the residue was distilled (110-112 C/10 Torr) to afford the target ketone (452 g, 63%) as thick, light yellow oil, which crystallized upon standing.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dimethyl-1H-pyrazole, its application will become more common.

Reference:
Article; Taydakov, Ilya V.; Krasnoselskiy, Sergey S.; Synthesis; vol. 45; 15; (2013); p. 2188 – 2192;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference of 694-48-4, The chemical industry reduces the impact on the environment during synthesis 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, I believe this compound will play a more active role in future production and life.

Put 100g (1.04mol, 1eq) of 1,3-dimethylpyrazole into the reaction bottleWith 400 mL of ethanol, 166.4 g (1.04 mol, 1.00 eq) of bromine was added dropwise with stirring at 5-10C.React at 5-10 for 4 hours,Sampling GC to check the remaining material is less than 1%, add 300mL water,Then add 200mL of saturated aqueous sodium thiosulfate solution to quench,Distilling ethanol under reduced pressure, cooling to 0 ,Filtered180.2g of 4-bromo-1,3-dimethyl-1H-pyrazole,GC purity 94.3%,The yield is 99%

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-pyrazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Xuzhou Shengyuan Chemical Co., Ltd.; Chen Hong; Yu Wanli; (8 pag.)CN111233768; (2020); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Synthetic Route of 694-48-4,Some common heterocyclic compound, 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, molecular formula is C5H8N2, 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.

In a three-necked reaction flask equipped with a stirrer, 50 ml of acetic anhydride and 12.7 g of nitric acid were added,1,3-dimethylpyrazole 9.7 g of acetic anhydride in 10 ml was slowly added dropwise to the mixed acid,Add 50-60 degrees after the end of the reaction until the reaction is complete,Cooled to room temperature to add 100 grams of ice water,Filtered and dried to give 12 g of 4-nitro-1,3-dimethylpyrazole,LC purity 80%, yield: 84%.

The synthetic route of 694-48-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Hande Chuanghong Biochemical Technology Co., Ltd.; Mao Zhongping; Ma Dongxu; Ge Yonghui; Ren Xuejing; Tan Jin; (9 pag.)CN106674116; (2017); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference of 694-48-4, These common heterocyclic compound, 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, 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.

Put 100g (1.04mol, 1eq) of 1,3-dimethylpyrazole into the reaction bottleAnd 800mL water and 400mL ethanol,Add in batches with stirring at room temperature132.1g (0.52mol, 0.5eq) of iodine,Subsequently, 84.8 g (0.624 mol, 0.6 eq) of 25% hydrogen peroxide was added dropwise at 15-20C.Stir at room temperature for 20 hours,Sampling GC to check the remaining material is less than 1%, add 200mL of saturated sodium bisulfite,Distilling ethanol under reduced pressure, cooling to 0, filteringget210.1g of 4-iodine-1,3-dimethyl-1H-pyrazole, GC purity 98.6%,The yield was 91%.

Statistics shows that 1,3-Dimethyl-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 694-48-4.

Reference:
Patent; Xuzhou Shengyuan Chemical Co., Ltd.; Chen Hong; Yu Wanli; (8 pag.)CN111233768; (2020); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 694-48-4, name is 1,3-Dimethyl-1H-pyrazole, 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 694-48-4, Recommanded Product: 1,3-Dimethyl-1H-pyrazole

In a three-necked reaction flask equipped with a stirrer, 50 ml of acetic anhydride and 12.7 g of nitric acid were added,1,3-dimethylpyrazole 9.7 g of acetic anhydride in 10 ml was slowly added dropwise to the mixed acid,Add 50-60 degrees after the end of the reaction until the reaction is complete,Cooled to room temperature to add 100 grams of ice water,Filtered and dried to give 12 g of 4-nitro-1,3-dimethylpyrazole,LC purity 80%, yield: 84%.

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