Month: September 2021

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. 98-18-0, name is 3-Aminobenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 98-18-0

A solution of 3-aminobenzenesulfonamide (271.9 mg, 1.58 mmol), 4,5- dichloro-2-fluoro-benzoic acid (300 mg, 1.43 mmol), and HATU (654.8 mg, 1.72 mmol) in DMF (3.12 mL) was treated with N-methylmorpholine (315.5 mu, 2.87 mmol) and stirred at 40 °C for 16 hours. The reaction was diluted with ethyl acetate and water and the organic layer separated. The organic layer was washed with 1 N HCl, water (3 x 50 mL), and brine, then dried over Na2S04, filtered, and concentrated. The residue was slurried in dichloromethane to form a white precipitate. The precipitate was filtered and washed with dichloromethane to provide 4,5-dichloro-2-fluoro-N-(3-sulfamoylphenyl)benzamide (422 mg, 81percent) as a white powder. 1H NMR (400 MHz, DMSO-d6) delta 10.85 (s, 1H), 8.32 – 8.25 (m, 1H), 8.03 (d, J = 6.7 Hz, 1H), 7.93 (d, J = 9.5 Hz, 1H), 7.83 (dt, J = 6.8, 2.2 Hz, 1H), 7.64 – 7.52 (m, 2H), 7.42 (s, 2H) ppm. ESI-MS m/z calc. 361.96948, found 364.7 (M+l)+; Retention time: 1.4 minutes (3 minutes run).

The synthetic route of 98-18-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; HADIDA-RUAH, Sara Sabina; ANDERSON, Corey; TERMIN, Andreas P.; BEAR, Brian Richard; ARUMUGAM, Vijayalaksmi; KRENITSKY, Paul; JOHNSON, James Philip; WO2015/10065; (2015); A1;,
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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. 758-96-3, name is N,N-Dimethylpropionamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C5H11NO

General procedure: To a stirred solution of 46 (800 mg, 2.71 mmol) in THF (20 mL) was slowly added n-BuLi (1.58 mol/L in n-hexane; 3.90 mL, 6.16 mmol) at -78 C under an argon atmosphere. After stirring for 1 h at the same temperature, N,N-dimethylpropionamide (0.890 mL, 8.10 mmol) was added in one portion at -78 C and the reaction mixture was allowed to gradually warm to room temperature over 3 h. The reaction was quenched with satd NH4Cl aq and the resulting mixture was extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (CHCl3) to give 47 (342 mg, 1.26 mmol, 46%) as a white solid.

The synthetic route of 758-96-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ochiai, Koji; Takita, Satoshi; Eiraku, Tomohiko; Kojima, Akihiko; Iwase, Kazuhiko; Kishi, Tetsuya; Fukuchi, Kazunori; Yasue, Tokutaro; Adams, David R.; Allcock, Robert W.; Jiang, Zhong; Kohno, Yasushi; Bioorganic and Medicinal Chemistry; vol. 20; 5; (2012); p. 1644 – 1658;,
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Some common heterocyclic compound, 33045-52-2, name is Methyl 2-methoxy-5-sulfamoylbenzoate, molecular formula is C9H11NO5S, 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. COA of Formula: C9H11NO5S

EXAMPLE 23 N-(1-cyclopentyl-2-pyrrolidinyl-methyl)-2-methoxy-5-sulphamoyl-benzamide 23 g of methyl 2-methoxy-5-sulphamoyl benzoate (0.09 mole) is dissolved hot, at about 90 C., in 115 ml of glycol in a 500 ml flask fitted with an agitator and a thermometer. The solution is cooled to 50 C. and the ester re-crystallises. 19 g of 1-cyclopentyl-2-amino-methyl-pyrrolidine is added. The suspension obtained is kept at 50 C. After 30 hours the ester is completely dissolved. The solution continues to be heated until a sample taken is found to be completely soluble in acetic acid. The solution is then cooled and the benzamide crystallises slowly. 150 ml of water is added and the precipitate is drained, washed with water and dried. 23 g (68%) of benzamide is obtained with a melting point of 147-148 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 33045-52-2, its application will become more common.

Reference:
Patent; Societe d’Etudes Scientifiques et Industrielle de l’Ile de France; US4673686; (1987); A;,
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Some common heterocyclic compound, 2832-19-1, name is 2-Chloro-N-(hydroxymethyl)acetamide, molecular formula is C3H6ClNO2, 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. Recommanded Product: 2832-19-1

Cresol was reacted with a-bromoisobutyric acid in the presence of NaOH to give acid 1, which was then amidomethylated using N-hydroxymethyl chloroacetamide inHOAc/H2SO4 to afford acid-amide 2. The amide was alcoholyzed in ethanol using HCI gas with concomitant ester formation to give the desired product Intermediate f. Intermediate f and Intermediate e were coupled together to form a compound of Example 1 in a manner similar to that described for the alternative route to Example 1 above.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2832-19-1, its application will become more common.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2005/49578; (2005); A1;,
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Reference of 141449-85-6, A common heterocyclic compound, 141449-85-6, name is tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate, molecular formula is C11H20N2O2, 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.

According to Synthetic Method 2: 2-bromo-4-methylthiazole-5-carboxylic acid ethyl ester (2.592 g, 10.36 mmol),Hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylic acid tert-butyl ester (2.000 g, 9.42 mmol), sodium carbonate (2.51 g, 23.6 mmol) and acetonitrile (40 mL) were added to a 100 mL reaction flask The reaction was carried out under reflux at 80 C for 4 hours.The reaction was completed by TLC and the reaction was stopped. Cool to room temperature, spin dry, purified by silica gel column ( petroleum ether / ethyl acetate (v / v) = 3 / 1), concentrated and dried to give the title compoundThe material was a pale yellow solid (2.70 g, yield: 75.1%).

The synthetic route of 141449-85-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jin Chuanfei; Xu Tengfei; Zhang Yingjun; Xue Yaping; (33 pag.)CN109956945; (2019); A;,
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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. 201162-53-0, name is 3-Boc-3,8-Diazabicyclo[3.2.1]octane, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Boc-3,8-Diazabicyclo[3.2.1]octane

tert-butyl 3,8- diazabicyclo[3.2.ljoctane-3-carboxylate (500 mg, 2.36 mmol) was dissolved in methanol (9 ml) for the addition of hydrochloric acid (4 M in dioxane, 2.95 mL, 11.8 mmol). The reaction mixture was stirred 16 h, then concentrated in vacuo and dried under high vacuum to afford the title compound (0.44 g, 2.38 mmol) in quantitative yield. LCMS MZ (M+H) 113.

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 201162-53-0.

Reference:
Patent; GENENTECH, INC.; CONSTELLATION PHARMACEUTICALS, INC.; ALBRECHT, Brian, K.; COTE, Alexandre; CRAWFORD, Terry; DUPLESSIS, Martin; GOOD, Andrew, Charles; LEBLANC, Yves; MAGNUSON, Steven, R.; NASVESCHUK, Christopher, G.; ROMERO, F. Anthony; TANG, Yong; TAYLOR, Alexander, M.; (271 pag.)WO2016/138114; (2016); A1;,
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These common heterocyclic compound, 6228-73-5, name is Cyclopropanecarboxamide, 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: 6228-73-5

Step 1 : 4-(Chloromethyl)-2-cyclopropylthiazole[0174] To a slurry of cyclopropanecarboxamide (10 g, 0.12 mol) in MTBE (150 rnL) was charged P2S5 (5 g, 12 mmol). The mixture was heated to 100 0C for 2 h (monitored by TLC, EtOAc/hexane 1 :1) and cooled to room temperature. Supernatant was decanted and concentrated to afford the intermediate thioamide (6 g, 56%) as a light yellow solid. MS (ES) m/z 102.1 (M+ H+)). This was suspended in acetone (100 mL) and charged with 1,3- dichloroacetone (7.0 g, 0.055 mol). The mixture was heated to reflux for 8 h (monitored by TLC, EtOAc/hexane 1 :1), cooled to room temperature and concentrated. The residue was purified by silica gel chromatography using 2 to 10% EtOAc in hexane to afford the title compound (8.0 g, 79%) as a light brown oil. 1H NMR (400 MHz, CDCl3) delta 7.02 (s, IH), 4.62 (s, 2H), 2.32 (m, IH), 1.16 (m, 2H), 1.05 (m, 2H). MS (ES) m/z 174.1 (M+ H+).

The synthetic route of Cyclopropanecarboxamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHEMOCENTRYX, INC.; CHEN, Xi; FAN, Pinchen; GLEASON, Mark, M.; JAEN, Juan, C.; LI, Lianfa; MCMAHON, Jeffrey, P.; POWERS, Jay; ZENG, Yibin; ZHANG, Penglie; WO2010/54006; (2010); A1;,
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Electric Literature of 1012884-46-6,Some common heterocyclic compound, 1012884-46-6, name is 11-Chloro-2-methyl-2,3-dihydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrol-1-one, molecular formula is C17H12ClNO2, 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.

Magnesium metal turnings (10 g) were added to a suspension of 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrol-1-one (7 g) in methanol (50 mL). The reaction mixture was slowly heated to refluxing temperature. Brisk effervescence was observed. The reaction mixture was cooled to control the reaction and again refluxed for about 2 hours. The reaction mass was diluted with methanol (30 mL), further refluxed for about 30 minutes, cooled to ambient temperature, slurried in water (150 mL) and filtered. pH of the filtrate was adjusted to 1-2 by adding concentrated hydrochloric acid. A clear solution was obtained. The solution was extracted with ethyl acetate (3x50mL) followed by washing with water (3×50 mL). Ethyl acetate was recovered to obtain a mixture of diastereomers as brown oil (4.6 g) followed by separation of the two isomers using silica gel column chromatography eluting with ethyl acetate-hexane mixture. cis-isomer: 50% trans-isomer 9%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 11-Chloro-2-methyl-2,3-dihydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrol-1-one, its application will become more common.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; ARYAN, Ram Chander; MISHRA, Anamika; NAIDU, Pudi, Giri, J.; SHARMA, Ramnik; WO2013/11461; (2013); A1;,
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These common heterocyclic compound, 79722-21-7, name is tert-Butyl benzyloxycarbamate, 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. Computed Properties of C12H17NO3

General procedure: Nucleophile (1-3 mol equiv), tris-(dibenzylideneacetone)dipalladium (2.5 mol %), tris-(2-furyl)phosphine (10 mol %) and potassium carbonate (2 mol equiv) were added to a solution of the aryl halide (1 mmol) in dry dimethylformamide (10 mL) in a Schlenk tube. The reaction mixture was then degassed using the freeze, pump, thaw (F.P.T.) technique (one cycle). Allene gas was then introduced at the required pressure (1 atm) and the Schlenk tube contents stirred and heated at 80 C for 16 h. After cooling and venting, DCM (20 mL) was added and the mixture filtered to remove inorganic salts. The filtrate was concentrated in vacuo and the residue was purified by column chromatography.

The synthetic route of tert-Butyl benzyloxycarbamate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Elboray, Elghareeb E.; Gao, Chuanjun; Grigg, Ronald; Tetrahedron; vol. 68; 14; (2012); p. 3103 – 3111;,
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Adding a certain compound to certain chemical reactions, such as: 169556-48-3, name is N-Boc-DL-valinol, 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 169556-48-3, SDS of cas: 169556-48-3

General procedure: An aldehyde (30 mmol), Zn(OTf)2 (13 mg, 35 mmol), and (N-Chloroethyl)morpholine HCl 6.5 mg, 35 mmol) were added to a 1dram vial. The dry solvent, acetonitrile (1mL), was added to the vial. Afterwards dipicolylamine (7 muL 35 mmol) was added to the vial and the vial was sonicated. Once the solution was transparent molecular sieves were added to the solution along with the respective alcohol (175 mmol). The assemblies were incubated for 16 h at room temperature in the dark.

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:
Article; Minus, Matthew B.; Featherston, Aaron L.; Choi, Sooyun; King, Sam C.; Miller, Scott J.; Anslyn, Eric V.; Chem; vol. 5; 12; (2019); p. 3196 – 3206;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics