Tag: M.W=100-200

617-36-7, name is Ethyl 2-amino-2-oxoacetate, 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. name: Ethyl 2-amino-2-oxoacetate

4′-Nitro-2-bromoacetophenone (6.100 g, 25 MMOL) and ethyl thioxamate (3.460 g, 26 MMOL) were dissolved in MeOH (20 mL) and the solution was refluxed for 1 h. After cooling to room temperature, the precipitated solid was collected by filtration, washed with cold MEOH and dried under vacuum (5.15 g, 75% yield).

The synthetic route of 617-36-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO KG; WO2004/65367; (2004); A1;,
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Reference of 108966-71-8, 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. 108966-71-8, name is 3,4-Difluorobenzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 500 mL round-bottomed flask fitted with a condenser and N2 inlet septum was placed a stir bar, 3, 4-difluoro-benzenesulfonamide (10 g, 52 mmol), anhydrous hydrazine (10. 56 mL, 336 mmol), and acetonitrile (180 mL). The mixture was refluxed for 6 h under N2. The solvent was then removed under vacuum and the residue was treated with H2O. The separated solid was filtered and washed with H20 to give the desired product. Exact mass calculated for C6H8FN302S 205. 03, found 206. 1 (MH+).

The synthetic route of 3,4-Difluorobenzenesulfonamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARENA PHARMACEUTICALS, INC.; WO2005/7658; (2005); A2;,
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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. 13304-62-6, name is N-Benzylacrylamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: N-Benzylacrylamide

General procedure: To a solution of 3-iodo-chromone (4 mmol) and olefin (4.8 mmol) in solvent was added catalyst (5 mmol %) and base (8 mmol). The reaction mixture was stirred via microwave heating under air. Then the mixture was poured into 10% HCl ice-water (300 mL) slowly with stirring. The suspension was filtered through a filter and filter cake was collected and dried. The crude product was purified by chromatography over silica gel to give resulting product.

The synthetic route of 13304-62-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Yikai; Lv, Zhiliang; Zhong, Hanyu; Zhang, Mingfeng; Zhang, Tao; Zhang, Wannian; Li, Ke; Tetrahedron; vol. 68; 47; (2012); p. 9777 – 9787;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 37394-93-7 as follows. Quality Control of 2-Chloro-N-(o-tolyl)acetamide

General procedure: A mixture of 5a-j (18 mmol) and KI (4.4 g, 27 mmol) inacetone (40 mL) was refluxed for 2 h, and the solvent was evaporated in vacuo. Water was added, and the solids were collected and dried to give compounds 6a-j.

According to the analysis of related databases, 37394-93-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhu, Xiong; Fu, Junjie; Tang, Yan; Gao, Yuan; Zhang, Shijin; Guo, Qinglong; Bioorganic and Medicinal Chemistry Letters; vol. 26; 4; (2016); p. 1360 – 1364;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 640-61-9 as follows. HPLC of Formula: C8H11NO2S

Add 0.2 mmol of N-methyl-p-toluenesulfonamide and a stirrer to a clean Schlenk reaction tube.Then, 1.0 mL of DMF solvent was added by syringe, and 1.0 mmol of NaOH was added to the reaction tube.Finally, 0.6 mmol of 1,1-dichloroethylene was added with a micro syringe, and the bottle was stoppered with a soft rubber stopper, and reacted at 70 C for 24 hours.TLC dot plate detection; after the reaction is completed, the reaction solution is added with ice water and extracted with ethyl acetate three times.The organic layer is concentrated and separated by column chromatography to obtain pure N-methyl-N-ethynyl p-toluenesulfonamide.White solid, yield 93%.

According to the analysis of related databases, 640-61-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangxi Normal University; Zhao Junfeng; Tu Yongliang; Zeng Xianzhu; (9 pag.)CN109320441; (2019); A;,
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Electric Literature of 120157-98-4,Some common heterocyclic compound, 120157-98-4, name is tert-Butyl acetylcarbamate, molecular formula is C7H13NO3, 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.

Carbonic acid (1 S,4f?)-4-(6-chloro-purin-9-yl)-cyclopent-2-enyl ester ethyl ester (1 equivalent), acetyl-carbamic acid terf-butyl ester (seeTanaka et al. (1988), supra; 1 .15 equivalents) and triphenyl phosphine (0.15 equivalents) were combined in an oven – dried flask under an atmosphere of argon. Dry deoxygenated THF (to 0.3 M with respect to carbonic acid (1 S,4f?)-4-(6-chloroiDurin-9-yl)-cyclopent-2-enyl ester ethyl ester) was added, followed by Pd2(dba)3 (5 mol%). The reaction mixture was stirred at 500C for 1 hour, and allowed to cool to room temperature, before the volatile components were removed under reduced pressure and the product purified by flash column chromatography/crystallization.

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

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2007/147659; (2007); A1;,
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Related Products of 4141-08-6, The chemical industry reduces the impact on the environment during synthesis 4141-08-6, name is 2-Amino-N-methylbenzamide, I believe this compound will play a more active role in future production and life.

To a suspension of A-2 (50 mg, 0.19 mmol) in 3 ml AcOEt (3 ml) at rt under an argon atmosphere were added 2-amino-N-methylbenzamide (29 mg, 0.19 mmol) and N-ethyl-diisopropylamine (0.1 ml, 0.59 mmol). The yellow suspension was cooled to 0 C. and propyl-phosphonic anhydride (50% in AcOEt, 0.31 ml, 0.48 mmol) was added. The suspension was stirred at 0 for 30 min and at rt overnight. The solvent was evaporated. The crude product was purified by silica gel chromatography using a CH2Cl2/MeOH gradient to provide the title compound (46 mg, 61%) as yellow solid.MS: M=389.2 (M+H)+

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-Amino-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bleicher, Konrad; Flohr, Alexander; Groebke Zbinden, Katrin; Gruber, Felix; Koerner, Matthias; Kuhn, Bernd; Peters, Jens-Uwe; Sarmiento, Rosa Maria Rodriguez; US2011/306589; (2011); A1;,
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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. 15441-10-8, name is 3-(Aminosulfonyl)propanoic acid, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C3H7NO4S

3-sulfamoylpropionic acid (Compound 1) (15.0 g, 97.94 mmol) and 2,4-dihydroxybenzoic acid (Compound 2)(10.2 g, 66.18 mmol) were dissolved in acetic anhydride (22.6 mL). Triethylamine (13.2 mL) was carefully addedto the mixture, andthe mixture was heated for 4 hr.After the reaction, it was cooled and diluted with water.The precipitated product was filtered and washed with aqueous methanol togive (7-hydroxy-2-oxo-2H-chromen-3-yl)methanesulfonamide (Compound 3), 21.2 g, yield 85%.

According to the analysis of related databases, 15441-10-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Zeng Qingqiang; (12 pag.)CN108586445; (2018); A;,
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Reference of 24243-71-8, 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. 24243-71-8, name is Propane-1-sulfonamide, This compound has unique chemical properties. The synthetic route is as follows.

To a 100-mL rm.md-hottom flask ‘.Vas added 2-[(1S,4S,5R)-5-[[5-cydopropyl-3-(2,6-dichorophenyl)-1 ,2-oxazol-4-yl]carbonyloxy ]-2-azahicyclol2.2.l]heptan-2-yl]-4-fluoro-l,3-benzothiazole-6-carboxylic acid I-1 (150 mg, 0.25 mmol, 1.0 equiv), dichloromethane (15mL), propane-1-sulfonamide (47 mg, 0.38 mmol, 1.5 equiv.), 4-dimethylaminopyridine (4715 mg, 0.38 mmoL 1.5 equiv), and EDC1 (73 mg, 0.38 mmol, 1.5 equiv) and the resultingmixture was stirred at room temperature for 16 h. 1 00 mL of brine was added and theaqueous mixture was extracted w·ith dichloromethane (l 00 mL x .5). The combined organicextracts ‘.vere dried over anhydrous sodium sulfate, filtered, and concentrated under reducedpressure. The residue was dissolved in 2 mL ofDMF and purified by Prep-HPLC using the20 follo·wing conditions: Column, XBridge C18 OBD Prep Column, 19 mm x 250 rnm; mobilephase, water (0 05% TFA) and ACN (68% to 84% over 8 min): Detector, UV 254 nm, toprovide 48.9 mg (28%) of(lS,4S,5R)-2-[4-fluoro-6-l(propane-l-sulfonyl)carbamoyl]-1,3-benzothiazol-2-y l]-2-azabicydo[2.2.1]heptan-5-y 5-cy dopropy l-3-(2,6-dichlorophenyl)-1 ,2-oxazole-4-carboxylate l-32 as a white solid. 1H NMR (300 MHz, CD30D) 8: 8.08 (d, J = 1.72.5 Hz, 1H), 7.70 — 7.49 (m, 4H), 5.00 (d, J ··· 6.6 Hz, lH), 4.41 (s, lH), 3.62—3.47 (m, 3H),3.23 (s, 1H), 3.00 (p, J 6.7 Hz, 1H), 2.60 (s, 1H), 2.25 (ddd, J 14. L 7.1, 2.5 Hz, lH),199- 1.78 (m, 2H), 1.71 (d, J = 10.6 Hz, HI), l.41- l.28 (m, 6H), 1.10 (t J = 7.5 Hz, 3H). MS (ES, m/z): [M+1l ” 693.25.

The chemical industry reduces the impact on the environment during synthesis Propane-1-sulfonamide. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ARDELYX, INC.; CHAO, Jianhua; JAIN, Rakesh; HU, Lily; LEWIS, Jason Gustaf; BARIBAULT, Helene; CALDWELL, Jeremy; (582 pag.)WO2018/39386; (2018); A1;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 125414-41-7 as follows. HPLC of Formula: C8H17NO4

The suspension of powdered KOH (3.05 g) and anhydrous THF (15 mL) was cooled to 0 C, Ar protection. Compound 2 (2.06 g) was dissolved in dry THF (10 mL) Was added dropwise to the reaction solution, After adding 0 reaction 15min, A solution of 4.7 mL of bromopropyne was added dropwise, 0 reaction 5min after the temperature to 35 C overnight, Deionized water (100 mL) was added, CH2Cl2 extraction, Saturated brine washing, Anhydrous Na2SO4 dried, filter, concentrate, Column separation, A yellow liquid 3 (2.467 g, 88%) was obtained.

According to the analysis of related databases, 125414-41-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangxi University; Wang, Mian; Wang, Jianyi; Chen, Zhengjun; (18 pag.)CN106554378; (2017); A;,
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Amide – an overview | ScienceDirect Topics