Tag: M.W=100-200

Related Products of 1129-26-6,Some common heterocyclic compound, 1129-26-6, name is 4-Methoxybenzenesulfonamide, molecular formula is C7H9NO3S, 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.

At room temperature, the appropriate amount of organic solvent (volume ratio of 1: DMAC 2 and the mixture of PEG-200), add, Compounds 200mmol formula (II), 15mmol lOOmmol catalyst into the formula (I), (Three mistakes to 12mmol chloride (A1C13) and 3mmol zinc iodide (Znl2) mixture), 80mmol oxidant Phi (TFA) 2,20mmol lOOmmol additives of niobium pentachloride and trifluoromethanesulfonic acid; and then warmed to 80 C, and the reaction was stirred at this temperature for 2 hours;After the [0046] reaction, the reaction system was cooled to room temperature, followed by addition of a saturated aqueous solution of sodium thiosulfate was sufficiently washed with acetone was added and extracted 3 times, the combined organic phase was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure , the residue by flash column chromatography on silica gel, ethyl acetate and an equal volume of petroleum ether mixture as eluent, to afford the compound of formula (III), in a yield of 96.9%

The synthetic route of 1129-26-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhang Wei; Zhang, Wei; (10 pag.)CN105294518; (2016); A;,
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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. 2896-98-2, name is Tetrahydro-1,4-thiazepan-5-one, A new synthetic method of this compound is introduced below., SDS of cas: 2896-98-2

To a solution of 1,4-thiazepan-5-one (3.0 g) in distilled THF (90 mL) cooled to 0 C. is added dropwise a solution of LiAlH4 in THF (1M solution, 22.9 mL). The mixture is stirred at room temperature for 2 h. The reaction is quenched by successive addition of water (2 mL), 15% NaOH (2 mL) and water (2 mL). The reaction mixture is filtered to remove the aluminum salt that had precipitated. The filtrate was dried (Na2SO4), filtered, and concentrated to obtain 2.63 g (98%) of 1,4-thiazepane as a yellow residue. Physical characteristics are as follows: 1H NMR (300 MHz, CDCl3) delta3.07, 2.96, 2.75, 1.92.

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; Pharmacia & Upjohn Company; US6248739; (2001); B1;,
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Synthetic Route of 10268-06-1, The chemical industry reduces the impact on the environment during synthesis 10268-06-1, name is 2-(2-Chlorophenyl)acetamide, I believe this compound will play a more active role in future production and life.

To a solution of compound methyl 2-(5-chloro-1–(2-fluoroethyl)-1H– indol?3?yl)?2-oxoacetate (200 mg, 0.710 mmol, 1.00 equiv.) and compound 2-(2-chlorophenyl)acetamide (132 mg, 0.780 mmol, 1.10 equiv.)in THF (10 mL, 0.071 M) was added with t-BuOK solution (190 mg, 1.69 mmol, 2.40 equivj/THF (5.00 mL) at 0 °C under nitrogen atmosphere. After the reaction mixture was stirred at 0 00 for another 5 h, it was quenched by iN HC1 (10.0 mL). The excess acid was neutralized by sodium bicarbonate. The solution was extracted with EtOAc (10 mL x3), washed with brine, dried with MgSO4, filtered, and concentrated in vacuo. The residue was purified through column chromatography using EtCAc:hexanes (1 : 1.5 (v/v)) to afford the title compound as a light yellow solid (64.8 mg, 0.161 rnm0l, 23percent yield). NMR Spectroscopy: ?H NMR (700 MHz, (CD3)2S0, 25 °C, ) : 11.22 (s, lH), 8.21 (s, lH), 7.58(d, J = 8.7 Hz, lH), 7.55 (d, J = 7.9 Hz, lH), 7.51?7.49 (m, 1H),7.41?7.40 (m, 2H), 7.13 (dd, J 2.0, 8.7 Hz, 1H), 6.19 (d, J 2.0Hz, 1H), 4.76 (t, J = 4.6 Hz, lH), 4.70 (t, J= 4.6 Hz, 1H), 4.65 (t,J 4.6 Hz, 1H), 4.60 (t, J = 4.6 Hz, 1H). 13C NMR (175 MHz, (CD3)2S0,25 °C, ) 171.7, 171.2, 135.7, 135.0, 134.2, 133.5, 132.2, 130.8,129.4, 127.6, 127.0, 126.2, 125.2, 122.2, 119.8, 112.4, 104.4, 83.0,82.0, 46.6 (d, J =19.9 Hz). Z9p NMR (376 MHz, (0D3)2S0, 25 °C, oe) -222.1 (m) . HRMS (ESI?TOF) (m/z) : calcd for C2flH14N2O2FC12 ( [M + H]),403.0416, found, 403.0408.

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, 2-(2-Chlorophenyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE RESEARCH FOUNDATION FOR THE STATE UNIVERSITY OF NEW YORK; NGAI, Ming-Yu; LEE, Katarzyna, N.; HU, Kongzhen; NASDEV, Neil; HAGGARTY, Stephen, J.; (120 pag.)WO2018/132636; (2018); 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. 518057-72-2, name is 5-Amino-2-fluorobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Amino-2-fluorobenzamide

To a well-stirred solution of 2-fluoro-5-aminobenzamide (43b)(0.20 g, 1.3 mmol) and 1-bromononane (0.30 g, 1.4 mmol) in ACN(20 mL) was added K2CO3 (0.25 g, 1.8 mmol). The reaction mixture was heated to reflux for 4 h. After the complete disappearance ofstarting material as indicated by TLC, the reaction mixture wassubjected to pass through a short pad of silica gel. The filtrate obtainedwas evaporated under reduced pressure and subjected topurification by flash column chromatography on silica gel. Thetitled compound (0.11 g) was obtained in 30% yield. 1H NMR(400 MHz, CDCl3) d 7.23e7.34 (m, 1H), 6.94 (d, J 8.8 Hz, 1H), 6.76(s, 1H), 6.62e6.71 (m, 1H), 6.28 (br. s., 1H), 3.70 (br. s., 1H), 3.11 (t,J 7.0 Hz, 2H),1.61 (quin, J 7.0 Hz, 2H),1.22e1.44 (m,12H), 0.89 (t,J 6.6 Hz, 3H); 13C NMR (101 MHz, CDCl3) d 165.6 (s, CONH2), 153.7(d, JCF 232 Hz, C2), 145.4 (d, JCF 2.0 Hz, C5), 120.1 (d, JCF 26 Hz,C1), 117.4 (d, JCF 9.1 Hz, C4), 116.5 (dd, JCF 12 Hz, C3), 114.3 (d,JCF 9.1 Hz, C6), 44.4, 31.9, 29.5, 29.4, 29.3, 27.1, 22.7, 14.1; LRMS(ESI) m/z 281 (M H, 100), 303 (M Na, 50); HRMS (ESI) calcdfor C16H26N2OF (M H) 281.2029, found 281.2033.

The synthetic route of 518057-72-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lui, Hok Kiu; Gao, Wei; Cheung, Kwan Choi; Jin, Wen Bin; Sun, Ning; Kan, Jason W.Y.; Wong, Iris L.K.; Chiou, Jiachi; Lin, Dachuan; Chan, Edward W.C.; Leung, Yun-Chung; Chan, Tak Hang; Chen, Sheng; Chan, Kin-Fai; Wong, Kwok-Yin; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 95 – 115;,
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Application of 98-18-0,Some common heterocyclic compound, 98-18-0, name is 3-Aminobenzenesulfonamide, molecular formula is C6H8N2O2S, 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 solution of 3-aminobenzenesulfonamide (1.0 g, 5.81 mmol) and pyridine (4.7 mL, 58.07 mmol) in dichloromethane (10.3 mL) at 0 C was added dropwise 2,5-difluorobenzoyl chloride (719.3 mu, 5.81 mmol). The mixture was allowed to warm to 25 C and was stirred for 72 hours. The reaction mixture was diluted with ethyl acetate and water. The layers were separated and the organic layer washed with brine (2x). The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give a clear oil that crystallized upon standing. The solid was re-dissolved in ethyl acetate and washed with IN HCl (3x). The organic layer was dried with MgS04, filtered and evaporated to yield 2,5-difluoro-N-(3-sulfamoylphenyl)benzamide (1.17 g, 64%) as a white solid. ESI- MS m/z calc. 312.04, found 313.3 (M+l) +; Retention time: 1.31 minutes (3 minutes run). 1H NMR (400 MHz, DMSO-d6) delta 10.81 (s, 1H), 8.31 (s, 1H), 7.84 (d, J = 9.1 Hz, 1H), 7.59 – 7.54 (m, 3H), 7.50 – 7.39 (m, 4H) ppm.

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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Adding a certain compound to certain chemical reactions, such as: 154350-29-5, name is Cyclopropanesulfonamide, 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 154350-29-5, Computed Properties of C3H7NO2S

Example 73Cyclopropanesulfonic acid [3,3-dimethyl-2-(4-morpholin-4-yl-phenyl)-l,2,3,4- tetrahydro-quinoline-6-carbonyl] -amideA mixture of 3,3-dimethyl-2-(4-morpholin-4-yl-phenyl)-l,2,3,4-tetrahydro-quinoline-6- carboxylic acid (70 mg, 0.19 mmol), l-3-dimethylaminopropyl-3-ethylcarbodiimide hydrochloride (55 mg, 0.29 mmol), 4-dimethylaminopyridine (35 mg, 0.29 mmol), cyclopropane sulfonamide (69 mg, 0.57 mmol) in dichloromethane (10 mL) was heated for at 65 °C for 12 hours. Removal of the solvent afforded an oil residue. Purification by Waters automated flash system (column: Xterra 30 mm x 100 mm, sample manager 2767, pump 2525, detector: ZQ mass and UV 2487, solvent system: acetonitrile and 0.1percent formic acid in water) afforded cyclopropanesulfonic acid [3,3-dimethyl-2-(4-morpholin-4-yl- phenyl)-l,2,3,4-tetrahydro-quinoline-6-carbonyl] -amide (24 mg, 27percent) as a light yellow solid: LC/MS m/e calcd for C25H31N3O4S (M+H)+: 470.6, observed: 470.3.

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

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; CHEN, Li; FENG, Lichun; HUANG, Mengwei; LIU, Yongfu; WU, Guolong; WU, Jim, Zhen; ZHOU, Mingwei; WO2011/128251; (2011); A1;,
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Related Products of 198989-07-0, These common heterocyclic compound, 198989-07-0, name is tert-Butyl 2,5-diazabicyclo[2.2.1]heptane-2-carboxylate, 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.

Example 825-[2-(2-Chloro-phenyl)-l-methyl-ethyl]-2,5-diaza-bicyclo[2.2.1]heptane-2- carboxylic acid (4-trifluoromethyl-phenyl)-amide (METHOD A)(i) l-Isocyanato-4-trifluoromethyl-benzene (990mg, 5.29mmol) was added to a stirred solution of 2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester (Ig, 5.04mmol) in dichloromethane (DCM) (20ml) and stirred overnight at room temperature. Trifluoroacetic acid (4ml) was added and stirred for 2h. The solution was made basic with 2N sodium hydroxide solution, separated, extracted with DCM and the combined organic extracts dried and evaporated. The residue was loaded onto a flash silica column, eluted with ethyl acetate to remove impurities followed by methanol/DCM (1:9) to elute the product. Evaporation gave 2,5-Diaza- bicyclo[2.2. lJheptane-2-carboxylic acid (4-trifluoromethyl-phenyl)-amide (905mg) as a brown solid.

Statistics shows that tert-Butyl 2,5-diazabicyclo[2.2.1]heptane-2-carboxylate is playing an increasingly important role. we look forward to future research findings about 198989-07-0.

Reference:
Patent; VERNALIS (R & D) LIMITED; WO2007/7069; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 90-16-4,Some common heterocyclic compound, 90-16-4, name is Benzo[d][1,2,3]triazin-4(3H)-one, molecular formula is C7H5N3O, 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: A suspension of 1,2,3-benzotriazin-4-one (II, 6 mmol), dibromoalkane (30 mmol), and potassium carbonate (1.66 g, 12 mmol) in acetone (50 mL) was refluxed for 8 h, and then cooled to room temperature. After removal of acetone by evaporation under reduced pressure, the residue was washed with water (100 mL) and extracted with CH2Cl2 (80 mL × 2). The organic layer was dried over anhydrous Na2SO4, concentrated and purified by flash chromatography on silica gel, eluting with petroleum ether (60-90 C)/EtOAc to afford 3-bromoalkyl-1,2,3-benzotriazin-4-one III in yields of 46-62%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Benzo[d][1,2,3]triazin-4(3H)-one, its application will become more common.

Reference:
Article; Zhang, Fan; Wu, Dang; Wang, Gao-Lei; Hou, Shuang; Ou-Yang, Ping; Huang, Jin; Xu, Xiao-Yong; Chinese Chemical Letters; vol. 28; 5; (2017); p. 1044 – 1048;,
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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. 113778-69-1, name is N-Methoxy-N-methylisobutyramide, A new synthetic method of this compound is introduced below., Product Details of 113778-69-1

A 250 mL flask was charged with a solution of 2-chloro-6-methoxypyridine (20 g, 0.139 mol, 1 equiv.) in THF (300 mL) under nitrogen atmosphere. To the mixture was then added tert-butyllithium (131 mL, 0.210 mol, 1.5 equiv.), which was added dropwise with stirring at -70 C. The reaction mixture was stirred at -78 C. for 2 h. N-methoxy-N-methylisobutyramide (24 g, 0.182 mol, 1.3 equiv.) was then added dropwise. The mixture was stirred for 3.0 h at -78 C. The reaction progress was monitored by LCMS. The reaction was quenched by the addition of ammonium chloride aqueous solution and then extracted with ethyl acetate, the organic layers combined and concentrated under vacuum. The residue was applied onto a sillia gel column with PE/EA=100/1 to yield 1-(6-chloro-2-methoxypyridin-3-yl)-2-methylpropan-1-one as yellow oil. Mass spectrum (ESI, m/z): Calculated for C10H12ClNO2, 214.1 (M+H), found 214.1.

The synthetic route of 113778-69-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Janssen Pharmaceutica NV; Zhang, Xuqing; Macielag, Mark J.; (179 pag.)US2019/47959; (2019); A1;,
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Some common heterocyclic compound, 16066-84-5, name is tert-Butyl methylcarbamate, molecular formula is C6H13NO2, 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. HPLC of Formula: C6H13NO2

24 g (120 mmol) of 2-chloro-5-(trifluoromethoxy)pyridine, 19.1 g (150 mmol) of tert-butyl N-methylcarbamate and 17.5 g (180 mmol) of sodium tert-butoxide were dissolved in 400 ml of toluene, 2.8 g (3 mmol) of tris(dibenzylideneacetone)dipalladium(0) and 1.73 g (3 mmol) of Xantphos were added under argon, and the mixture was stirred at 100-105 C. for 12 h. Subsequently, the mixture was filtered through Celite and the solvent was distilled off under reduced pressure.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 16066-84-5, its application will become more common.

Reference:
Patent; BAYER CROPSCIENCE AKTIENGESELLSCHAFT; FISCHER, Ruediger; HAGER, Dominik; HOFFMEISTER, Laura; KAUSCH-BUSIES, Nina; WILCKE, David; WILLOT, Matthieu; GOeRGENS, Urich; ILG, Kerstin; MOSRIN, Marc; PORTZ, Daniela; TURBERG, Andreas; US2018/305353; (2018); A1;,
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Amide – an overview | ScienceDirect Topics