Category: 133228-21-4

These common heterocyclic compound, 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, 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. SDS of cas: 133228-21-4

17(1) 1-(Dimethylsulfamoyl)-5-(2-chloro-6-methylphenylthio)pyrazole 32.3 ml of a 1.59M solution of butyllithium in hexane were added, at -78 C. and under an atmosphere of nitrogen, to a solution of 8.18 g of 1-(dimethylsulfamoyl)pyrazole [prepared as described in Example 1(1)] in 250 ml of dry tetrahydrofuran, and the resulting mixture was allowed to stand at the same temperature for 40 minutes. At the end of this time, a solution of 14.73 g of 2-chloro-6-methylphenyl disulfide in 100 ml of tetrahydrofuran was added to the mixture, which was then stirred at the same temperature for 1 hour. The reaction mixture was then mixed with an aqueous solution of ammonium chloride and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which it was concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, eluted with a 10:1 by volume mixture of hexane and ethyl acetate, to give 13.70 g (yield 88%) of the title compound as an oil. Nuclear Magnetic Resonance Spectrum (CDCl3, 200 MHz), delta ppm: 7.48 (1H, doublet, J=1.6 Hz); 7.45-7.27 (3H, multiplet); 5.32 (1H, doublet, J=1.6 Hz); 3.05 (6H, singlet); 2.53 (3H, singlet).

The synthetic route of N,N-Dimethyl-1H-pyrazole-1-sulfonamide has been constantly updated, and we look forward to future research findings.

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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C5H9N3O2S

N,N-dimethyl-lH-pyrazole-l -sulfonamide (8.89 g, 50.8 mmol) was dissolved in anhydrous THF (250 mL). The solution was cooled at -78C, a solution of n-butyl lithium (32.6 mL, 81.4 mmol, 2.5 M in hexane) was added dropwise, and then the mixture was stirred for 45 minutes. A solution of hexachloroethane (18.0 g, 76.3 mmol) in anhydrous THF (20 mL) was added dropwise at -78C, and the reaction stirred for 1.5 hours. Water was added, and the mixture was extracted 5 times with dichloromethane. The combined organic phases were washed with brine and then dried over magnesium sulfate. After evaporation of the solvent, 5-chloro-N,N- dimethyl-lH-pyrazole-1 -sulfonamide was obtained and used in the next step without further purification.

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.

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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, This compound has unique chemical properties. The synthetic route is as follows., name: N,N-Dimethyl-1H-pyrazole-1-sulfonamide

To a solution [OF N-DIMETHYLSULFAMOYLPYRAZOLE] (44.0 g, 0.251 mol) in dry tetrahydrofuran (500 mL) at-78 C was added dropwise a solution of n-butyllithium (2.5 M in hexane, 105.5 mL, 0.264 mol) while maintaining the temperature [BELOW-60 C.] A thick solid formed during the addition. Upon completion of the addition the reaction mixture was maintained for an additional 15 minutes, after which time a solution of 1,2-dibromo- tetrachloroethane (90 g, 0.276 mol) in tetrahydrofuran (150 mL) was added dropwise while maintaining the temperature below-70 [C.] The reaction mixture turned a clear orange; stirring was continued for an additional 15 [MINUTES. THE-78 C] bath was removed and the reaction was quenched with water (600 mL). The reaction mixture was extracted with methylene chloride (4x), and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride-hexane (50: 50) as eluent to afford the title product as a clear colorless oil (57.04 g). 1H NMR [(CDC13)] [8] 3.07 (d, 6H), 6.44 (m, 1H), 7.62 (m, 1H).

According to the analysis of related databases, 133228-21-4, the application of this compound in the production field has become more and more popular.

Related Products of 133228-21-4, 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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

19(1) 1-(Dimethylsulfamoyl)-4-fluoropyrazole 2.1 liters of fluorine gas (10% in N2) were bubbled, at 0-5 C., into a solution of 11.1 g of 1-(dimethylsulfamoyl)pyrazole [prepared as described in Example 1(1)] and 25.9 g of sodium acetate in 500 ml of a 9:1 by volume mixture of chloroform and acetic acid. The mixture was stirred for 2 hours, after which it was diluted with water. The organic layer was separated, washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, eluted with a 5:1 by volume mixture of hexane and ethyl acetate, to give 1.77 g (yield 14%) of the title compound as an oil.

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, N,N-Dimethyl-1H-pyrazole-1-sulfonamide, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, 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 133228-21-4, Safety of N,N-Dimethyl-1H-pyrazole-1-sulfonamide

Step 2: Preparation of 3-bromo-pyrazole-l-sulfonic acid dimethylamide; Pyrazole-1-sulfone acid dimethylamide (17.6 g) was dissolved in dry THF (200 mL) and cooled to -78C. A solution of n-butyllithium (80 mL, 1.3 M) was added slowly over a period of 15 min and stirred for further 15 min at – 78C. A solution of 1, 2-dibromo-l, 1, 2 , 2-tetrachloroethane(35.8 g) in dry THF (60 mL) was added within 10 min to this solution and stirred for further 15 min at -78C, then the cool bath was removed and the mixture was quenched with water after stirring for 1 h. The reaction mixture was extracted 3x with ethyl acetate, the combined org. layers were washed with brine, dried over MgSO4 and concentrated in vacuum.The residue was purified by column chromatography (silica gel 60, hexane/ethyl acetate = 5:1, Rf = 0.25) to afford 21.3 g of the title compound of the formulae2 as a colorless oil.1H-NMR (CDCl3, TMS) delta (ppm) : 3.08 (6H, s) , 6.43 (IH, m) , 7.61 IH, m) .

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

Step A: Preparation of 3~bromo-N,N-dimethyl-lH-pyrazole-l-sulfonamide; To a solution of N,N-dimethylsulfamoylpyrazole (44.O g, 0.251 mol) in dry tetrahydrofuran (500 mL) at -78 0C was added dropwise a solution of n-butyllithium (2.5 M in hexane, 105.5 mL, 0.264 mol) while maintaining the temperature below -60 C. A thick solid formed during the addition. Upon completion of the addition the reaction mixture was stirred at -78 C for an additional 15 minutes, after which time a solution of 1,2-dibromo- tetrachloroethane (90 g, 0.276 mol) in tetrahydrofuran (150 mL) was added dropwise while maintaining the temperature below -70 0C. The reaction mixture turned a clear orange; stirring was continued for an additional 15 minutes. The -78 0C bath was removed and the reaction was quenched with water (600 mL). The reaction mixture was extracted with methylene chloride (4x), and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride-hexane (50:50) as eluent to afford 57.04 g of the title product as clear colorless oil. 1H NuMR (CDCl3): delta 7.62 (m,lH), 6.44 (m,lH), 3.07 (d,6H).

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.

Related Products of 133228-21-4,Some common heterocyclic compound, 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, molecular formula is C5H9N3O2S, 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 S1 (25.3 g, 144 mmol) in THF (200 mL) at -78 C was added dropwise 1.6 M n-butyllithium in hexane (99 ml, 159 mmol). After 30 min, EtI (12.8 mL, 159 mmol) was added dropwise. The reaction mixture was stirred at -78 C for 30 min and allowed to room temperature. After 1 h, the stirring became difficult by formation of white precipitates. THF (200 mL) was added dropwise to give yellow solution. The stirring was continued for 2 h. Then, the mixture was poured into saturated NaHCO3 aq. (600 mL), and extracted with EtOAc (400 mL x2), and the extract was dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (n-hexane/EtOAc,100:0 to 30:70, v/v) to afford S2 (19.8 g, 68%) as colorless liquid.1H NMR (300 MHz, CDCl3) d 1.30 (3H, t, J = 7.8 Hz), 2.94 (2H, dd, J = 15.0, 7.5 Hz), 3.03 (6H, s), 6.13 (1H, br s), 7.55 (1H, br s).

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