Category: amides-buliding-blocks

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. 19047-31-5, name is 2-Chloro-N-cyclopropylacetamide, A new synthetic method of this compound is introduced below., Product Details of 19047-31-5

Compound m (148 mg) was dissolved in 5.0 ml DMF and Cs2CO3 (330 mg) was added, followed by the addition of N1-cyclopropyl-2-chloroacetamide (130 mg). The vial was capped and the reaction was heated to 70 C. in a heat block for 4 hrs. The reaction was completed by LCMS. Diluted reaction with H2O, extracted with EtOAc, dried over MgSO4, concentrated by vacuum, and flashed by ISCO (EtOAc/hexanes) to give compound o. Compound o was dissolved in 10 ml THF and cooled to 0 C. before adding 0.14 ml 2.5 M LAH in THF. The reaction was stirred 1 hr 35 min at 0 C. and was completed by LCMS. The reaction was quenched with 400 uL 10% NaOH and 400 uL EtOH, diluted with H2O and 1 M HCl, extracted with DCM, dried over MgSO4 and concentrated under vacuum to give compound p. Compound p was dissolved in 2 ml 1.0 M TBAF in THF and 3 ml THF and heated to 60 C. overnight. Reaction was completed by LCMS and diluted with H2O, extracted with EtOAc, washed with brine, dried over MgSO4, concentrated under vacuum and purified by HPLC to give 18 mg of the final compound 85.

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; Rawson, Thomas E.; Safina, Brian; Dotson, Jennafer; Zhou, Aihe; Aliagas-Martin, Ignacio; Halladay, Jason; Liang, Jun; Rueth, Matthias; Zhu, Bing-Yan; US2007/37791; (2007); A1;,
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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. 6973-09-7, name is 5-Amino-2-methylbenzenesulfonamide, A new synthetic method of this compound is introduced below., Safety of 5-Amino-2-methylbenzenesulfonamide

Example 4b: Synthesis of Pazopanib Hydrochloride (0040) To a suspension of N-(2-chloropyrimidin-4-yl)-N-2,3-trimethyl-2H-indazol-6-amine (90 g, 0.312 mol) and 5-amino-2-methyl benzene sulfonamide (64.07 g, 0.344 mol) in isopropyl alcohol (900 mL) was added 4M hydrochloric acid solution in isopropyl alcohol (1.56 mL, 6.25 mol). The reaction mixture was heated to reflux temperature for 10 hours to 12 hours. The reaction mixture was cooled to 25 C. The reaction mixture was further stirred at 25 C. to 30 C. for 30 minutes, then the solid was filtered. The wet solid was washed with isopropyl alcohol (180 mL×2), and then dried under vacuum at 45 C. to 50 C. for 12 hours to afford the hydrochloride salt of 5-({4-[(2,3-dimethyl-21-I-indazol-6-yl)(methyl) amino] pyrimidin-2-yl} amino-Z-methylbenzene sulfonamide as a light brown solid. Yield: 97% w/w.

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

Reference:
Patent; Sun Pharmaceutical Industries Limited; KUMAR, Rajesh; GIRI, Prabhat; BARMAN, Dhiren C.; NATH, Asok; PRASAD, Mohan; (5 pag.)US2015/329526; (2015); A1;,
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Reference of 79722-21-7, A common heterocyclic compound, 79722-21-7, name is tert-Butyl benzyloxycarbamate, molecular formula is C12H17NO3, 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.

Sodium hydride 60% dispersion in mineral oil (0.55 g, 13.7 mmol) was added portion- wise to a stirring solution of fe/f-Butyl /V-(benzyloxy)carbamate (2.05 g, 9.18 mmol) in DMF (15 mL) under a nitrogen atmosphere at ambient temperature. The reaction mixture was stirred for 15 min. 1 (3.00 g, 10.1 mmol) in DMF (10 mL) was added dropwise and the reaction mixture was stirred under a nitrogen atmosphere at ambient temperature overnight. The reaction mixture was quenched with water (100 mL) and extracted with ethyl acetate (3 x 100 mL). The organic layers were pooled, washed with brine (100 mL), dried over Na2S04 and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 1 :4 ethyl acetate/hexane to give a yellow oil (Yield: 1 .94 g, 37%). (0296) 1 H NMR (400 MHz, CDCI3): : delta 7.78 – 7.82 (m, 2H), 7.65 – 7.70 (m, 2H), 7.29 – 7.37 (m, 5H), 4.77 (s, 2H), 3.87 (t, J = 7.2 Hz, 2H), 3.69 (t, J = 7.2 Hz, 2H), 3.60 – 3.62 (m, 2H), 3.54 – 3.57 (m, 2H), 1.45 (s, 9H); 13C NMR (101 MHz, CDCI3): delta 168.3, 156.8, 135.8, 134.1 , 132.3, 129.6, 128.6, 128.5, 123.4, 81 .5, 77.1 , 67.7, 67.3, 49.8, 37.5, 28.4.

The synthetic route of 79722-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE UNIVERSITY OF SYDNEY; CODD, Rachel; KATSIFIS, Andrew; LIFA, Tulip; TIEU, William; RICHARDSON-SANCHEZ, Tomas; (90 pag.)WO2017/96430; (2017); A1;,
Amide – Wikipedia,
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Related Products of 1280210-80-1, The chemical industry reduces the impact on the environment during synthesis 1280210-80-1, name is MK-3102 interMediate3, I believe this compound will play a more active role in future production and life.

Step A: tert-Butyl { (2R.3S,5R)-2-(2,5-difluorophenyl)-5- [2-(methylsulfonyl)-2,6- dihydropyrrolo [3 ,4-c]pyrazol-5(4H)-yl]tetrahydro-2H-pyran-3-yl } carbamateA vessel was charged with N,N-dimethylacetamide (520.6 kg), 2-(methylsulfonyl)-2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-5-ium benzenesulfonate (intermediate 2, 30.0 kg, 86.8 mol), and tert-butyl [(2R,35)-2-(2,5-difluorophenyl)-5-oxotetrahydro-2H-pyran-3 -yl]carbamate (intermediate 1, 31.2 kg, 95.3 mol). After dissolving at room temperature, the solution was cooled to 0-10 C and sodium triacetoxyborohydride (24 kg, 113 mol) was added in four equalportions every 40 mm. The reaction was then allowed to warm to room temperature and stirred an additional 5h. The solution was then cooled to 5-15 C and water (672 kg) was added over 1- 2h. The resulting slurry was filtered and the cake washed sequentially with N,Ndimethylacetamide, twice with water, and then n-heptane. The solids were dried under vacuum at 40-60 C to give tert-butyl { (2R,3S,5R)-2-(2,5-difluorophenyl)-5 – [2-(methylsulfonyl)-2,6-dihydropyrrolo [3 ,4-cjpyrazol-5(41])-yljtetrahydro-2H-pyran-3-yl } carbamate.

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, MK-3102 interMediate3, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ARROYO, Itzia; KRUEGER, Davida; CHEN, Ping; MOMENT, Aaron; BIFTU, Tesfaye; SHEEN, Faye; ZHANG, Yanfeng; MERCK SHARPE & DOHME LTD.; WO2013/3249; (2013); A1;,
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Application of 683-57-8, The chemical industry reduces the impact on the environment during synthesis 683-57-8, name is 2-Bromoacetamide, I believe this compound will play a more active role in future production and life.

Example 25; 2-[4-({|2-(trifluoroniethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide; [0234] To a suspension of N-piperidin-4-yl-2-(trifluoromethyl)benzenesulfonamide hydrochloride salt, example 3, (74 mg, 0.21 mmol) in acetone was added potassium iodide (catalytic amount) and bromoacetamide (33 mg, 0.23 mmol). The reaction mixture was heated (500C, 16 h) and monitored by LCMS. The solvent was removed in vacuo and water was added. The product was extracted with ethyl acetate and concentrated to dryness. The crude residue was purified by flash chromatography using asolvent system comprised of dichloromethane and 10% methanolic dichloromethane (0 to 80%). The isolated free base was dissolved in ethyl acetate and treated with HCl gas to afford the hydrochloride salt of 2- [4-({[2-(trifluoromethyl)phenyl]sulfonyl}amino)piperidin-l-yl]acetamide (72 mg, 85%).[0235] MS (ESI+) m/z 366;HPLC purity 100.0%, Rtau 4.6 minutes;HRMS: calculated for C4H18F3N3O3S + H+, 366.10937; found (ESI, [MH-H]+), 366.1075;

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-Bromoacetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; WYETH; WO2008/61016; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2895-21-8, name is N-Isopropyl-2-chloroacetamide, 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 2895-21-8, Application In Synthesis of N-Isopropyl-2-chloroacetamide

A mixed solution of the compound 1 (120 mg), the compound 2 (123 mg), and sodium carbonate (96 mg) in acetonitrile (5 mL) was stirred for 22 hours at 50C under argon atmosphere. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water and saturated brine, and dried over Chem Elut (registered trademark). The solvent was distilled off under reduced pressure, and the resultant residue was purified by silica gel column chromatography (eluent: chloroform-ammonia water (10% methanol solution) = 90:10). The resultant residue was triturated with a mixed solvent of hexane-ethyl acetate to give the compound 3 (95 mg) as a pale yellow solid. MS (APCI) 365 [M+H]+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-Isopropyl-2-chloroacetamide, and friends who are interested can also refer to it.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; SAKAKIBARA, Ryo; USHIROGOCHI, Hideki; SASAKI, Wataru; ONDA, Yuichi; YAMAGUCHI, Minami; AKAHOSHI, Fumihiko; (69 pag.)EP3381904; (2018); A1;,
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Amide – an overview | ScienceDirect Topics

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. 39549-79-6, name is 2-Amino-4-methylbenzamide, A new synthetic method of this compound is introduced below., Quality Control of 2-Amino-4-methylbenzamide

General procedure: Sodium hydrogen sulfite (4 mmol) was added to a solution of anthranilamide 1 (2 mmol) and benzaldehyde 2 (2 mmol) in N,N- dimethylacetamide (5 mL). The mixture was heated under continuous stirring at 150 o C for 2-3 h and poured into ice water. The precipitate was then filtered, washed with water followed byethanol, and dried to yield the 2-arylquinazolinones 3-31.#10;#10;

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; Khadka, Daulat Bikram; Tran, Giap Huu; Shin, Somin; Nguyen, Hang Thi Minh; Cao, Hue Thi; Zhao, Chao; Jin, Yifeng; Van, Hue Thi My; Chau, Minh Van; Kwon, Youngjoo; Le, Thanh Nguyen; Cho, Won-Jea; European Journal of Medicinal Chemistry; vol. 103; (2015); p. 69 – 79;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 459817-82-4, name is tert-Butyl 1,2,3-oxathiazolidine-3-carboxylate 2,2-dioxide, This compound has unique chemical properties. The synthetic route is as follows., Safety of tert-Butyl 1,2,3-oxathiazolidine-3-carboxylate 2,2-dioxide

Example 10 (2S)-1-{[2-(5-Brom-2,3-dihydro-indol-1-yl)-ethylamino]-acetyl}-pyrrolidine-2-carbonitrile, Hydrochloride Salt This compound was made from 5-brom-2,3-dihydroindole, 2,2-dioxo-[1,2,3]oxathiazolidine-3-carboxylic acid tert-butyl ester according to example 5, steps A] to C]. The hydrochloride salt of the title compound was obtained according to example 2. MS (ISP): 399.3 (MNa+), 377.3 (MH+). 1H-NMR (DMSO-d6): 2.05 (m, 2H), 2.17 (m, 2H); 2.94 (t, 2H), 3.16(m, 2H), 3.38 (m, 5H), 3.60 (m, 1H), 4.00-4.30 (m, 5H), 4.85 (t, 1H), 6.55 (d, 1H), 7.20 (d, 2H), 7.21 (s, 1H), 9.10 (broad s, 2H). (+Rotamer).

According to the analysis of related databases, 459817-82-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer, Markus; Hunziker, Daniel; Kuehne, Holger; Loeffler, Bernd M.; Sarabu, Ramakanth; Wessel, Hans P.; US2003/130281; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 53844-02-3, 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. 53844-02-3, name is Benzyl (2-bromoethyl)carbamate, This compound has unique chemical properties. The synthetic route is as follows.

Sodium hydride (60%, 120mg, 3.0mmol) was added to a solution of 2-tert-butoxycarbonylamino-3-fluorobenzoic acid methyl ester from Example 20A (750mg, 2.8mmol) in DMF (8.0ml) while cooling in an ice/water bath. The mixture was allowed to warm to room temperature and stirred for 30min. (2-bromoethyl)carbamic acid benzyl ester (360mg, 2.8mmol) and sodium iodide (420mg, 2.8mmol) were added and the mixture was heated at 65C for 18h. The mixture was cooled and evaporated in vacuo. The residue was partitioned between EtOAc and brine and the organic layer was dried and evaporated in vacuo. The residue was purified by flash chromatography on silica (EtOAc:pet. ether 30:70) to give a colourless gum; yield 340mg, 27%.

The chemical industry reduces the impact on the environment during synthesis Benzyl (2-bromoethyl)carbamate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; FERRING B.V.; WO2006/18443; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 57957-24-1, name is N-(1-Phenylvinyl)acetamide, 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 57957-24-1, Safety of N-(1-Phenylvinyl)acetamide

General procedure: A reaction tube was charged with N-acetylenamide 1a (100 mg, 0.636 mmol), alkyne 2a (124 mg, 0.699 mmol), Cu(OAc)2.H2O (126 mg, 0.636 mmol), KPF6 (23.4 mg, 0.127 mmol) and [RuCl2(p-cymene)]2 (7.8 mg, 0.0127 mmol). To that, DME or water (3 mL) was added by syringe. The reaction mixture was stirred at 110 C under N2 as indicated time in the table 1.The reaction mixture was cooled down to rt, diluted with 10 mL of DCM. The mixture was then filtered through Celite. The combined organic portion was washed with water, then dried over MgSO4 and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel with hexane/ethyl acetate as eluent to yielded the desired pyrrole 3a (202 mg, 0.605 mmol) in 95% yield. Products obtained in this work were characterized by spectral methods particularly with 1H, 13C NMR, and ESI-Mass analyses, further, the data were compared with those reported.

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-(1-Phenylvinyl)acetamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Murugan, Kaliyappan; Liu, Shiuh-Tzung; Tetrahedron Letters; vol. 54; 21; (2013); p. 2608 – 2611;,
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