Month: March 2021

Application of 214210-30-7, 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. 214210-30-7, name is 4-Bromo-2-fluorobenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Sodium ethoxide (0.546 mL, 6.61 mmol) is dissolved in DMF (11 mL.). 4-Bromo-2- fluorobenzenesulphonamide (1.20 g, 4.72 mmol ) in DMF (5 mL) is added dropwise. The RM is stirred at RT for 1 h, then the temperature is raised to 60 C for 2h. Sodium ethoxide (0.39 mL, 4.72 mmol) is added and the RM is stirred for another hour. The RM is partitioned between EtOAc and water. The organic phase is washed with water and brine, dried over MgSC , filtered and evaporated under reduced pressure. The crude is purified by FC (H/EtOAc from 0:100 to 50:50), to afford the title compound as a white powder (841 mg, 64%). LC-MS A: tR = 0.78 min; no ionization.

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, 4-Bromo-2-fluorobenzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; FRETZ, Heinz; LYOTHIER, Isabelle; POTHIER, Julien; RICHARD-BILDSTEIN, Sylvia; SIFFERLEN, Thierry; WYDER PETERS, Lorenza; POZZI, Davide; CORMINBOEUF, Olivier; (306 pag.)WO2017/85198; (2017); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 72505-21-6, 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. 72505-21-6, name is 4-(Trifluoromethyl)thiobenzamide, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 4-(trifluoromethyl)benzothioamide 1 (10 mmol/2.05 g) in the minimum required quantity of absolute ethanol (10 mL), ethyl 2-chloroacetoacetate 2 (15 mmol/2.46 g) was added and the resulting mixture was heated on the water bath for 5 h. The solution was cooled down and neutralized with a solution of potassium carbonate. The resulting solid was filtered, washed with water, recrystallized from ethanol to give the target compound.

The chemical industry reduces the impact on the environment during synthesis 4-(Trifluoromethyl)thiobenzamide. I believe this compound will play a more active role in future production and life.

Reference:
Article; Nastasa, Cristina; Tiperciuc, Brindusa; Duma, Mihaela; Benedec, Daniela; Oniga, Ovidiu; Molecules; vol. 20; 9; (2015); p. 17325 – 17338;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 103361-99-5, name is 7-Fluoro-2H-benzo[b][1,4]oxazin-3(4H)-one, 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 103361-99-5, HPLC of Formula: C8H6FNO2

To a solution of 7-fluoro-4H-benzo[1,4]oxazin-3-one (3.00 g, 17.95 mmol) in concentrated H2SO4 (12 mL) at -10 C. was added a mixture of fuming nitric acid (1.131 g, 17.95 mmol, 0.75 mL) and concentrated H2SO4 (0.75 mL) dropwise, keeping the internal temperature below 0 C. After addition, the reaction mixture was stirred at -10 C. for 10 min. The reaction mixture was poured onto crushed ice (200 g) with care. The precipitate was collected by filtration, washed with water (50 mL) and dried in vacuo to give 7-fluoro-6-nitro-4H-benzo[1,4]oxazin-3-one as a light yellow solid (3.5 g, 92%). 1H NMR (DMSO-d6, 400 MHz): delta 11.02 (s, 1H), 7.61 (d, J=7.6 Hz, 1H), 7.23 (d, J=12.0 Hz, 1H), 4.77 (s, 2H).

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; Wang, Jianfei; Breinlinger, Eric C.; Barth, Martine; Friedman, Michael M.; Guillier, Fabrice; Argiriadi, Maria A.; Edmunds, Jeremy; Potin, Dominique; Hobson, Adrian D.; Wu, Wentao; Bonafoux, Dominique; Thomas, Didier; George, Dawn M.; Dai, Linlin; Zhang, Yang; US2014/206663; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 758-96-3, 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. 758-96-3 name is N,N-Dimethylpropionamide, 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.

Weigh 4-methylbenzothiazole (0.5mmol, 75mg), K2S2O8 (2mmol, 0.54g) and Eosin Y (0.01mmol, 6.5mg) in a 25mL Schlenk reaction tube,Then add N, N-dimethylpropionamide (38mmol, 3.8g), put it under the LED white light of 20W power to react, stir the reaction at room temperature, monitor the progress of the reaction with TLC, the reaction ends after 24h, and the reaction solution is concentrated The solvent was removed, and the concentrated solution was separated by column chromatography (eluent: petroleum ether / ethyl acetate with a volume ratio of 5: 1) to obtain a yellow oil, that is, the derivative Im. The yield was 72%.

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

Reference:
Patent; Zhejiang University of Technology; Weng Jianquan; Xu Wenxiu; Dai Xiaoqiang; Liu Xinghai; (11 pag.)CN110432282; (2019); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 5238-56-2, The chemical industry reduces the impact on the environment during synthesis 5238-56-2, name is N-(2-Hydroxyethyl)methacrylamide, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of glycosyl donor10 1 (0.635 gm, 1 mmol), glycosyl acceptor 10b (0.142 g 1.1 mmol) and 4 A molecular sieves powder (100 mg) in anhydrous CH2Cl2 (10 mL) was added AuBr3 (0.031 g, 0.07 mmol) under argon atmosphere at room temperature. The reaction mixture was stirred at room temperature for the specified time and the completion of the reaction is judged by TLC analysis. The reaction mixture was filtered through Celite and the filtrate was concentrated in vacuo to obtain a crude residue which was purified by conventional silica gel column chromatography using ethyl acetate-petroleum ether as mobile phase to obtain compound 11b.

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-(2-Hydroxyethyl)methacrylamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Thadke, Shivaji A.; Kar, Mritunjoy; Gupta, Sayam Sen; Hotha, Srinivas; Carbohydrate Research; vol. 346; 12; (2011); p. 1511 – 1518;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 17641-08-6,Some common heterocyclic compound, 17641-08-6, name is 2-Chloro-N-(3-methoxyphenyl)acetamide, molecular formula is C9H10ClNO2, 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.

General procedure: To a stirred solution of substituted aniline (1 mmol) and chloroacetyl chloride (1 mmol) which was stirred in 5 mL DMF for 20 min, were added benzyl amine derivatives (1.3 mmol) and CS2 (5 mmol). The reaction mixture was allowed to stir for required additional time (Table 2). Then, 5 mL of water was added and the solution was extracted with ethyl acetate and dried over sodium sulfate and purified by passing over a silica gel column chromatography using petroleum ether/ethyl acetate (8:2).

The synthetic route of 17641-08-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sadat-Ebrahimi, Seyed Esmail; Karim, Leila; Moghimi, Setareh; Yahya-Meymandi, Azadeh; Mahdavi, Mohammad; Vosooghi, Mohsen; Foroumadi, Alireza; Shafiee, Abbas; Journal of Sulfur Chemistry; vol. 38; 1; (2017); p. 43 – 51;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

366-49-4, name is 2-Acetamido-4-fluorotoluene, belongs to amides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 366-49-4

A solution of 5-fluoro-2-methylaniline (25 g, 200 mmol) in toluene (250 mL) was treated with Ac2O (25 mL, 226 mmol) and heated at reflux for 1 h. The reaction mixture was concentrated in vacuo when a colorless solid precipitated out which was filtered and washed with ether and hexanes. The colorless solid was taken in acetic acide (150 mL) and treated with a solution of Br2 (9.6 mL, 186 mmol) in acetic acid (20 mL) and stirred at rt for 12 h. The reaction mixture was diluted with water when a colorless solid 17 (40 g, 81.6%) precipitated out. It was filtered and extensively washed.

The synthetic route of 366-49-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkatraman, Srikanth; Velazquez, Francisco; Gavalas, Stephen; Wu, Wanli; Chen, Kevin X.; Nair, Anilkumar G.; Bennett, Frank; Huang, Yuhua; Pinto, Patrick; Jiang, Yueheng; Selyutin, Oleg; Vibulbhan, Bancha; Zeng, Qingbei; Lesburg, Charles; Duca, Jose; Heimark, Larry; Huang, Hsueh-Cheng; Agrawal, Sony; Jiang, Chuan-Kui; Ferrari, Eric; Li, Cheng; Kozlowski, Joseph; Rosenblum, Stuart; Shih, Neng-Yang; George Njoroge; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 447 – 458;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 6973-09-7,Some common heterocyclic compound, 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, molecular formula is C7H10N2O2S, 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.

2-Chloro-5-fluoro-N4-[4-(prop-2-ynyloxy)phenyl]-4-pyrimidineamine (0.514 g, 1.85 mmol), 3-(aminosulfonyl)-4-methylaniline (0.689 g, 3.70 mmol, made by reduction of commercially available 2-methyl-5-nitrobenzenesulfonamide or synthesized as described below), and trifluoroacetic acid (0.186 mL, 2.41 mmol) were combined with iPrOH (6.0 mL) in a sealed vial and heated at 100¡ã C. for 3 h. The reaction mixture was cooled to room temperature and diluted with 1N HCl (80 mL). N2-(3-Aminosulfonyl-4-methylphenyl)-5-fluoro-N4-[4-(prop-2-ynyloxy)phenyl]-2,4-pyrimidinediamine (I) was isolated as a white solid by suction filtration (0.703 g). 1H NMR (DMSO-d6): delta 10.08 (bs, 2H), 8.19 (d, J=4.5 Hz, 1H), 7.89 (s, 1H), 7.74 (dd, J=2.4 and 8.4 Hz, 1H), 7.58 (d, J=8.7 Hz, 2H), 7.32 (bs, 2H), 7.23 (d, J=8.4 Hz, 1H), 6.97 (d, J=8.4 Hz, 2H), 4.79 (d, J=2.1 Hz, 2H), 3.59-3.55 (m, 1H), 2.53 (s, 3H); LCMS: purity: 97percent; MS (m/e): 428 (MH+).

The synthetic route of 6973-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rigel Pharmaceuticals, Inc.; Magilavy, Daniel; US2014/73659; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 34813-49-5, name is 2-Methylpropane-2-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. Product Details of 34813-49-5

General procedure: Inside a N2 filled glovebox, benzenesulfonamide (250 mg, 1.590 mmol) and copper(I) iodide (15.14 mg, 0.080 mmol), 4-toluene bromide (326mg, 1.91 mmol), potassium carbonate (550 mg, 3.98 mmol), Acetonitrile (4 mL), and N1,N2dimethylethane-1,2-diamine (70.1 mg, 0.795 mmol) was charged into a vial. The vial was then heated to 70 oC for 8hr, LC indicated >97% conversion of benzenesulfonamide. The reaction mixture was then cooled to room temperature. 2N HCl (4mL) was added slowly, followed by EtOAc extraction (5mL x 3). The organic layers were combined, concentrated, and flash chromatographed (SiO2, 20:1–> 3:1 Heptane:EtOAc) to give N(p-tolyl) benzene sulfonamide as white solids (380 mg, 97%).

The synthetic route of 2-Methylpropane-2-sulfonamide has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Xiang; Guram, Anil; Ronk, Michael; Milne, Jacqueline E.; Tedrow, Jason S.; Faul, Margaret M.; Tetrahedron Letters; vol. 53; 1; (2012); p. 7 – 10;,
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. 7700-07-4, name is N,N-Dimethylethenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of N,N-Dimethylethenesulfonamide

General procedure: A dried 25 ml, screw-sealed tube was charged with degassed [1,4 dioxane/water, 3 ml, 99:1 (v/v)], followed by the addition of 6 (140 mg, 1 mmol) and 3-chlorophenylboronic acid (624 mg, 4 mmol). After addition of [RhOH(cod)]2 (2 mol %, 9.1 mg, 0.02 mol) and rac-BINAP (6 mol %, 37 mg, 0.06 mol), the tube was closed. After removing air by vacuum the tube was back-filled with nitrogen and heated in a pre-heated oil bath at 120 C for 18 h. After cooling to room temperature, the resulting mixture was diluted with EtOAc (5 ml) and extracted with 5% aqueous NaHCO3 solution (5 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude obtained 7 was further purified by flash chromatography [silica gel 60 (0.040-0.063 nm, Merck)] eluent, Et2O-petroleum ether (40-60), 3:1 (v/v) or CH2Cl2 – EtOAc,, 95:5 (v/v), to give 158 mg of pure 7 (64%).

The synthetic route of 7700-07-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zilaout, Hicham; Van Den Hoogenband, Adri; De Vries, Jelle; Lange, Jos H.M.; Terpstra, Jan Willem; Tetrahedron Letters; vol. 52; 45; (2011); p. 5934 – 5939;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics