Category: 3144-09-0

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. 3144-09-0, name is Methylsulfonamide, A new synthetic method of this compound is introduced below., Product Details of 3144-09-0

General procedure: According to the Scheme 1, 4 mmol of N-(4-Sulfamoylphenyl) acetamide was treated with acetic anhydride (4 mmol) in glacial acetic acid (10 mL). The mixture was stirred at 50C for the predetermined time. The progress of the reaction was monitored by TLC analysis. After the completion of the reaction, the precipitate was collected by filtration and washed with water. The impure precipitate was dissolved in aqueous solution of sodium carbonate (50 mL, pH=8.0) and filtered. Acetic acid was gently added to the liquor dropwise to precipitate the product (pH=5.0). The precipitate was collected by filtration to afford N-(4-acetamidophenylsulfonyl)acetamide a1 as the white solid (0.97 g, 95%). The catalytic activities of different heterogeneous catalysts were determined by reactions performed in THF using a 1:1 molar ratio of sulfonamide to acetic anhydride or benzoyl chloride. In a typical route, N-(4-sulfamoylphenyl) acetamide (4 mmol) was treated with acetic anhydride (4 mmol) in the presence of catalyst (0.1 g) in THF (10 mL). After the appropriate time, the catalyst was separated with an external magnetic field, the solvent was evaporated by rotary evaporator. The precipitate was dissolved in aqueous solution of sodium carbonate (50 mL, pH=8.0) and filtered. Acetic acid was gently added to the liquor dropwise to precipitate the product (pH=5.0). The precipitate was collected by filtration and was washed with distilled water to afford N-(4-acetamidophenylsulfonyl)acetamide as the white solid (0.95 g, 93%).

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; Ghasemi, Mohammad Hadi; Kowsari, Elaheh; Hosseini, Seyed Kiumars; Tetrahedron Letters; vol. 57; 3; (2016); p. 387 – 391;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 3144-09-0, name is Methylsulfonamide, belongs to amides-buliding-blocks 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 3144-09-0, COA of Formula: CH5NO2S

To a 500 mL row1d bottom f1ask vas added a solution of methanesulfonamide (1 0 g,105.13 mmol, l.OO equiv.) in dichloromeHume (300 mL) follo¡¤wed by TEA (22 g, 217.4120 mmol, 1.50 equiv.), Boc20 (27.5 g, 126.00 mmoL 1.20 equiv.), and 4-dimethylaminopyridine(1.28 g, 10.48 mmol, 0.10 equiv.). The reaction mixture v.¡¤as stirred at room temperatmeovernight and then concentrated under vacuurn. 200 mL ofFhO vvas added, the pFf value of the solution was adjusted to 3 using a 1M hydrogen chloride aqueous solution, and thernixture was extracted with ethyl acetate (200 mL x 3). The combined organic extracts werew¡¤ashed vvith brine (300 mL x 2), dried over anhydrous sodium sulfate and concentratedunder vacuum to give oftert-butyl N-methanesulfonylcarbamate 216b (10.06 g, 49%) as a5 ¡¤white solid.

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, Methylsulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARDELYX, INC.; CHAO, Jianhua; JAIN, Rakesh; HU, Lily; LEWIS, Jason Gustaf; BARIBAULT, Helene; CALDWELL, Jeremy; (582 pag.)WO2018/39386; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

The chemical industry reduces the impact on the environment during synthesis 3144-09-0, name is Methylsulfonamide, I believe this compound will play a more active role in future production and life. 3144-09-0

To a 50 mL three-necked flask, add 1.22 g (10.0 mmole) of benzoic acid and 12 mL of chloroform and stir at room temperature for about 5 minutes. Thereafter, the internal temperature was adjusted to around 5 C. by cooling with external cooling in an ice water bath, and then 1.484 g (5.0 mmole) of triphosgene and 3.036 g (30 mmole) of triethylamine were added in turn, (10.0 mmole) of methanesulfonamide was added thereto, and the mixture was stirred for about 5 minutes. Then, the ice water bath was removed and the temperature was raised to room temperature. While stirring for about 1 hour, the reaction was carried out by thin film chromatography (TLC) After confirming the completion of the reaction, the reaction solvent was distilled off under reduced pressure, and 15 mL of water was added to the resulting solid to dissolve the solid salt formed by the neutralization reaction of triethylamine and hydrochloric acid produced as a by-product The desired compound, acylsulfonamide, is dispersed in a solid form and stirred. After filtration, the filtrate was washed with water, and the obtained solid was dried to obtain 1.89 g (yield: 94.9%) of acyl sulfoneamide as a target compound in a solid form.

The chemical industry reduces the impact on the environment during synthesis 3144-09-0. I believe this compound will play a more active role in future production and life.

Reference:
Patent; HANKYONG NATIONAL UNIV. Industry-University Cooperation Foundation; Kim Mi-su; Han Gi-jong; (8 pag.)KR2017/136043; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3144-09-0, 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. 3144-09-0, name is Methylsulfonamide, This compound has unique chemical properties. The synthetic route is as follows.

In a 2-liter reaction flask, 1 liter of ethyl acetate and 66 grams of methylsulfonamide were added, and 109 grams of chloroacetyl chloride was gradually added; the temperature was gradually increased to 65C for 12 hours until the end of the reaction.The reaction solution gradually cooled to 0 degree, and a large amount of white solid precipitated; it was filtered and dried to obtain 112 g of solid SLP-10b (X=Cl).Yield: 94%.H NMR (400MHz, CDCl3): delta 4.02 (s, 2H), 3.28s, 3H)ESI/MS+(m/z):171

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.

Reference:
Patent; Shanghai Aikangrui Pharmaceutical Technology Co., Ltd.; Fan Linfeng; Zhu Yangwei; Qiu Aiyun; Lv Bojie; Xu Zhonghui; Zhang Changxuan; (11 pag.)CN106316967; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3144-09-0, These common heterocyclic compound, 3144-09-0, name is Methylsulfonamide, 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.

Add in the reaction flask2- (4 – ((5,6-diphenylpyrazin-2-yl) (isopropyl) amino) butoxy) acetic acid (S-I)(21.0 g, 0.05 mol), carbonyldiimidazole (12.2 g, 0.075 mol) andDichloromethane (210 mL), heated to reflux for 1 hour,The temperature was lowered to 20-30 C, methanesulfonamide (9.5 g, 0.10 mol)After stirring for 10 minutes, triethylamine (10.1 g, 0.10 mol)Continue to react for 5 hours. Water (50 mL) was added,Dropping 1N hydrochloric acid to adjust the pH of the system to 5-6, liquid separation,The organic phase was washed with water (50 mL ¡Á 2), dried over anhydrous sodium sulfate,Filtration, the filtrate was concentrated under reduced pressure Sai Xip crude(Purity: 99.16%, HPLC chromatogram shown in Figure 1),The crude product was recrystallized from absolute ethanol (270 mL) to give a white solid racemic solution(24.0 g, yield: 96.8%, purity: 99.93%,HPLC chromatogram shown in Figure 2).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 3144-09-0.

Reference:
Patent; Hangzhou East China Pharmaceutical Group New Drug Institute Co., Ltd.; Zhang Qianqian; Qu Xiaoxia; (14 pag.)CN107365275; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 3144-09-0, name is Methylsulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 3144-09-0

e) Boc-N-(4-Benzylsulfanyl-5-nitro-thiophen-3-ylmethyl)-methanesulfonamide Triethylamine (22.0 mL, 158 mmol), di-tert-butyl dicarbonate (27.5 g, 126 mmol), and 4-(N,N-dimethylamino)pyridine (1.28 g, 10.5 mmol) were added sequentially to a solution of methanesulfonamide (10.0 g, 105 mmol) in dichloromethane (300 mL) at 25 C. The mixture was stirred at 25 C. for 2 h, and then was concentrated in vacuo to ~40 mL volume. Ethyl acetate (350 mL) was added and the mixture was washed with 1.0 M aqueous hydrochloric acid solution (300 mL). The aqueous layer was extracted with ethyl acetate (250 mL) and the combined organic layers were dried over sodium sulfate, filtered and were concentrated in vacuo to afford Boc-N-methanesulfonamide (17.1 g, 87.6 mmol, 83%) as a white solid. 1H NMR (400 MHz, CDCl3) delta: 1.53 (9H, s), 3.27 (3H, s).

The synthetic route of 3144-09-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anadys Pharmaceuticals, Inc.; US2009/306057; (2009); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

3144-09-0, 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. 3144-09-0, name is Methylsulfonamide, A new synthetic method of this compound is introduced below.

A solution of Boc20 (41.2 g, 189.2 mmol) in DCM (200 mL) was added dropwise to a stirred suspension of methane sulfonamide (15.0 g, 157.7 mmol), Et3N (23.6 mL, 173.5 mmol) and DMAP (1.9 g, 15.8 mmol) in DCM (200 mL). The resulting suspension was stirred for 3 h at room temperature and concentrated under vacuum. The resulting residue was diluted with EtOAc (300 mL) and acidified with 1 N HCI (200 mL). The organic layer was washed with water followed by brine, dried over Na2S04 and concentrated under reduced pressure to obtain a crude mixture, which was triturated with 10% EtOAc in petroleum ether to obtain B1 as a white solid (25.0 g, 81 %). Rf: 0.6 (50% EtOAc in petroleum ether). LCMS m/z = 194.3 (M – H). 1H NMR (400 MHz, CDCI3): delta 1.44 (s, 9H), 3.19 (s, 3H), 7.19 (s, 1 H).

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; PFIZER INC.; CHEKLER, Eugene Lvovich Piatnitski; GILBERT, Adam Matthew; UNWALLA, Rayomand Jal; VERHOEST, Patrick Robert; ANDERSON, James Thomas; WO2015/181676; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 3144-09-0, name is Methylsulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 3144-09-0

Reference Example 42 To a mixture of methane sulfonamide (1.96 g), triethylamine (3.2 mL), 4-(dimethylamino)pyridine (252 mg), and dichloromethane (30 mL) was added a mixture of di-tert-butyl dicarbonate (5.17 g) and dichloromethane (40 mL) at room temperature for 30 minutes. The mixture was concentrated after stirring for 2 hours, and the residue was distributed with ethyl acetate and 1 N hydrochloric acid. The organic layer was washed with water, dried and concentrated. The obtained residue was purified by silica gel column chromatography to obtain tert-butyl methylsulfonyl carbamate (2.44 g). 1H-NMR (300 MHz, CDCl3) delta: 1.52 (9H, s), 3.28 (3H, s).

The synthetic route of 3144-09-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1553074; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics