Category: 133228-21-4

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., Recommanded Product: 133228-21-4

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 dichloromethane [(4X)] and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using dichloromethane-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).

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:
Patent; E.I. DU PONT DE NEMOURS AND COMPANY; WO2004/11447; (2004); A2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

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.

To a solution of N,N-dimethyl-1H-pyrazole-1-sulfonamide obtained in Step A (6.74 g) in tetrahydrofuran (75 mL) was added dropwise n-butyllithium hexane solution (1.3 M, 31.1 mL) over 15 min at -78C. The reaction mixture was stirred at -78C for 15 min, and a solution of 1,2-dibromo-1,1,2,2-tetrachloroethane (13.8 g) in tetrahydrofuran (25 mL) was added dropwise thereto over 10 min. The reaction mixture was stirred at -78C for 15 min, and then at room temperature for 1 hr. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (8.03 g). 1H NMR (400 MHz, CDCl3) delta 3.06 (6H, s), 6.42 (1H, d, J = 1.6 Hz), 7.60 (1H, d, J = 1.6 Hz)

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.

Reference:
Patent; Takeda Pharmaceutical Company Limited; NAGAMIYA, Hiroyuki; YOSHIDA, Masato; SETO, Masaki; MARUI, Shogo; ODA, Tsuneo; ISHICHI, Yuji; SUZUKI, Hideo; KUSUMOTO, Tomokazu; YOGO, Takatoshi; RHIM, Chul Yun; YOON, Cheolhwan; LEE, Gil Nam; KANG, Hyun Bin; KIM, Kwang Ok; JEON, Hye Sun; EP2818473; (2014); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

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., Computed Properties of C5H9N3O2S

Step B: Preparation of 3-chloro-N,N-dimethyl-1H-pyrazole-1-sulfonamide. Under a nitrogen atmosphere, a solution of N,N-dimethyl-1H-pyrazole-1-sulfonamide (5.0 g, 28 mmol) (i.e. the product of Example 12, Step A) in tetrahydrofuran (50 mL) was cooled to -78 0C and then treated with n-butyllithium (2 M solution in cyclohexane, 15.0 mL, 30 mmol) dropwise. The reaction mixture formed a thick precipitate, and stirring was continued for 30 minutes after the addition. To the stirred suspension, a solution of hexachloroethane (7.1 g, 30 mmol) in tetrahydrofuran (20 mL) was added dropwise. After 30 minutes the resulting clear solution was warmed to ambient temperature and quenched with the addition of water (70 mL). The reaction mixture was extracted with dichloromethane and dried over MgSO4. The reaction mixture was filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (50 % hexanes in dichloromethane as eluant) to give 1.71 g of 5-chloro-iV,iV-dimethyl-lH-pyrazole- EPO 1 -sulfonamide. The S-chloro-MiV-dimethyl-lH-pyrazole-l-sulfonamide was heated to 110 C for 12 h with a catalytic amount of pyrazole to isomerize to the title compound. 1H NMR (CDCl3) 5 3.07 (s, 6H), 6.33 (s, IH), 7.60 (s, IH).

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.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2007/14290; (2007); A2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

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, Formula: C5H9N3O2S

Step A: Preparation of3-Bromo-N,N-dimethyl- 1 H-pyrazole- 1-sulfonamide To a solution of N-dimethylsulfamoylpyrazole (44.0 g,0.25 1 mol) in dry tetrahydrofuran (500 mE) at 78 C. wasadded dropwise a solution of n-butyllithium (2.5 M inhexane,105.5 mE, 0.264 mol) while maintaining the temperaturebelow 60 C. A thick solid formed during the addition. Uponcompletion of the addition the reaction mixture was maintained for an additional 15 minutes, afier which time a solution of 1 ,2-dibromotetrachloroethane (90 g, 0.276 mol) intetrahydroffiran (150 mE) was added dropwise while maintaining the temperature below .-70 C. The reaction mixtureturned a clear orange; stirring was continued for an additional15 minutes. The 78 C. bath was removed and the reactionwas quenched with water (600 mE). The reaction mixture wasextracted with methylene chloride (4x), and the organicextracts were dried over magnesium sulfate and concentrated.The crude product was further purified by chromatography onsilica gel using methylene chloride/hexane (50:50) as eluentto afford the title product as a clear colorless oil (57.04 g).?H NMR (CDC13) oe 3.07 (d, 6H), 6.44 (m, 1H), 7.62 (m,1H).

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

Reference:
Patent; E I DU PONT DE NEMOURS AND COMPANY; Berger, Richard Alan; Annan, Isaac Billy; Lahm, George Philip; Flexner, John Lindsey; Selby, Thomas Paul; Stevenson, Thomas Martin; US9173400; (2015); B2;,
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. 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

Step A: Preparation of3-Chloro-N,N-dimethyl- 1 H-pyrazole- 1-sulfonamideTo a solution of N-dimethylsulfamoylpyrazole (188.0 g,1.07 mol) in dry tetrahydrofuran (1500 mE) at 78 C. wasadded dropwise a solution of 2.5 M n-butyllithium (472 mE,1.18 mol) in hexane while maintaining the temperature below65 C. Upon completion of the addition the reaction mixturewas maintained at 78 C. for an additional 45 minutes, afterwhich time a solution of hexachloroethane (279 g, 1.18 mol)in tetrahydrofuran (120 mE) was added dropwise. The reac40 tion mixture was maintained for an hour at 78 C., warmedto 20 C. and then quenched with water (1 E). The reactionmixture was extracted with methylene chloride (4×500 mE);the organic extracts were dried over magnesium sulfate andconcentrated. The crude product was further purified by chro45 matography on silica gel using methylene chloride as eluentto afford the title product compound as a yellow oil (160 g).?HNMR(CDC13) oe 3.07 (d, 6H), 6.33 (s, 1H), 7.61 (s, 1H).

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:
Patent; E I DU PONT DE NEMOURS AND COMPANY; Berger, Richard Alan; Annan, Isaac Billy; Lahm, George Philip; Flexner, John Lindsey; Selby, Thomas Paul; Stevenson, Thomas Martin; US9173400; (2015); B2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference 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.

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 synthetic route of 133228-21-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E.I. DUPONT DE NEMOURS AND COMPANY; WO2006/68669; (2006); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

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, category: pyrazoles-derivatives

12. 3-Ethyl-pyrazole-l-sulphonic acid dimethylamideTo a solution of pyrazole-1-sulphonic acid dimethylamide (13. Ig, 74.9 mmol) in anhydrous tetrahydrofuran (100 ml) at -78 0C under a nitrogen atmosphere was added dropwise a solution of n-butyl lithium in hexanes (1.6M, 51 ml, 82.3 mmol). The reaction was stirred thus for 30 minutes then iodoethane (6.6 ml, 82.4 mmol) was added dropwise. The reaction mixture was allowed to warm to room temperature then stirred thus over the weekend. EPO Water was then added and the solution was extracted with ethyl acetate. The separated organic liquors were washed with brine, dried (MgSO4) and concentrated to furnish the title compound as a yellow/ brown oil (12.6g, 85%).

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.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; THE INSTITUTE OF CANCER RESEARCH: ROYAL CANCER HOSPITAL; ASTRAZENECA AB; WO2006/136829; (2006); A2;,
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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., Product Details of 133228-21-4

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 dichloromethane [(4X)] and the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using dichloromethane-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).

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:
Patent; E.I. DU PONT DE NEMOURS AND COMPANY; WO2004/11447; (2004); A2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Reference of 133228-21-4, The chemical industry reduces the impact on the environment during synthesis 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, I believe this compound will play a more active role in future production and life.

To a solution of N,N-dimethylsulfamoylpyrazole (44.0 g, 0.251 mol) in dry tetrahydrofuran (500 ml) at -78C was added dropwise a solution of n-butyllithium (2.5 M in hexane, 105.5 ml, 0.264 mol) while maintaining the temperature below -60C. 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-dibromotetrachloroethane (90 g, 0.276 mol) in tetrahydrofuran (150 ml) was added dropwise while maintaining the temperature below -70C. The reaction mixture turned a clear orange; stirring was continued for an additional 15 minutes. The -78C 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 NMR (CDCl3): delta 3.07 (d, 6H), 6.44 (m, 1H), 7.62 (m, 1H).

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.

Synthetic Route 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.

Step A: Preparation of 3-Chloro-N,N-dimethyl-1H-pyrazole-1-sulfonamideTo a solution of N-dimethylsulfamoylpyrazole (188.0 g, 1.07 mol) in dry tetrahydrofuran (1500 mL) at -78 C. was added dropwise a solution of 2.5 M n-butyllithium (472 mL, 1.18 mol) in hexane while maintaining the temperature below -65 C. Upon completion of the addition the reaction mixture was maintained at -78 C. for an additional 45 minutes, after which time a solution of hexachloroethane (279 g, 1.18 mol) in tetrahydrofuran (120 mL) was added dropwise. The reaction mixture was maintained for an hour at -78 C., warmed to -20 C. and then quenched with water (1 L). The reaction mixture was extracted with methylene chloride (4×500 mL); the organic extracts were dried over magnesium sulfate and concentrated. The crude product was further purified by chromatography on silica gel using methylene chloride as eluent to afford the title product compound as a yellow oil (160 g). 1H NMR (CDCl3) delta 3.07 (d, 6H), 6.33 (s, 1H), 7.61 (s, 1H).

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.