Month: March 2021

Related Products of 112257-19-9, These common heterocyclic compound, 112257-19-9, name is tert-Butyl methyl(2-(methylamino)ethyl)carbamate, 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.

Preparation Example 1-3: Preparation of Compound (II-4)[0060][0061] Under an argon stream, 4-((S)-2-((S)-2-(6-(2,5-dioxo-2,5-dihydro-1H-pyrrol-1-yl)hexanamido)-3-methylbutanamido)-5-ureidopentanamido)benzyl (4-nitrophenyl) carbonate (6.8 g, 9.22 mmol) was dissolved in 150 mL of anhydrousdimethylformamide, and stirred, together with t-butyl methyl(2-(methylamino)ethyl)carbamate (1.82 g, 9.68 mmol) at 20- 25¡ãC for 19 hrs. After completion of the reaction, the reaction mixture was completely concentrated in a high vacuum,and the concentrate was purified by silica gel column chromatography to obtain an amino-protected derivative of compound (II-4) (5.14 g, 71percent).[0062]1H NMR (400 MHz, DMSO-d6) delta0.78-0.8 (d, 3 H), 0.8-0.83 (d, 3 H), 1.09 -1.99 (m, 10 H), 1.33 (s, 9 H), 1.92(m, 1 H), 2.07-2.19 (m, 2H), 2.66-2.73 (d, 3H), 2.8-2.81 (m, 3H), 2.9-3.0 (m, 2H), 3.37 (m, 2 H), 4.15 (t, 1 H), 4.34 (m,1 H), 4.94 (s, 2 H), 5.38 (s, 2 H), 5.94 (brt, 1 H), 6.96 (s, 2H), 7.23 (d, 2 H), 7.55 (d, 2 H), 7.77 (d, 1 H), 8.04 (d, 1 H),9.95 (brs, 1 H)[0063] LC-MS m/z: 787.5 [M+H]+[0064] With the exception of using the amino-protected derivative of compound (II-4), the same procedure as inPreparation Example 1-2 was repeated to obtain a concentrated TFA salt of the title compound.

The synthetic route of 112257-19-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Celltrion, Inc.; PARK, Young Jun; JEONG, Jin-kyo; CHOI, Young Mi; LEE, Minseob; KIM, Yeon Jung; KIM, Kyoung Suk; CHOI, Joon hun; LEE, Jin Seo; CHO, Eun Joo; SONG, Hyunnam; PARK, Sung Jun; LEE, Jong-hyoup; LEE, Matthew Sangyup; LEE, In-Suk; KIM, Joon woo; HONG, Seung Suh; EP2927227; (2015); A1;,
Amide – Wikipedia,
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. 2835-68-9, name is 4-Aminobenzamide, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Aminobenzamide

General procedure: A solution of 3a-e (2 mmol) in10 mL THF was added slowly to a cooled solution of 4,6-dichloro-5-nitropyrimidine (0.43 g, 2.2 mmol) and TEA (0.20 g, 2 mmol) in THF (20 mL), and mixture was stirred for about 30 min at 0 C. Stirring was continued for 4 h at room temperature and the reaction was monitored by TLC. The reaction mixture was added into 60 mL H2O, and extracted with EA (50 mL ¡Á 2). The combined organic extract was washed with brine, dried over anhydrous Na2SO4, and concentrated in vacuo to get the crude product which was next purified by column chromatography on silica employing ethyl acetate/petroleum ether as eluted to obtain the pure product to give the product 3a-e.

The synthetic route of 2835-68-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yu, Xu-Ri; Tang, Yun; Wang, Wen-Jing; Ji, Sen; Ma, Shuang; Zhong, Lei; Zhang, Chun-Hui; Yang, Jiao; Wu, Xiao-Ai; Fu, Zheng-Yan; Li, Lin-Li; Yang, Sheng-Yong; Bioorganic and Medicinal Chemistry Letters; vol. 25; 22; (2015); p. 5449 – 5453;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 24167-52-0,Some common heterocyclic compound, 24167-52-0, name is 3-Chloro-N,N-dimethylbenzamide, molecular formula is C9H10ClNO, 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.

N’-cyanobenzimidamide (16.8 g, 115 mmol), Compound 2-4-2 (21 g, 115 mmol) and phosphorus oxychloride (12 mL, 128 mmol) were added to 500 mL of acetonitrile and then stirred under reflux for 1 hour. After cooling to room temperature, the resulting solid was filtered, washed with water and ethanol, and then dried to produce Compound 2-4-3 (27.6 g, yield: 80%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Chloro-N,N-dimethylbenzamide, its application will become more common.

Reference:
Patent; LG CHEM, LTD.; KANG, Min Young; PARK, Tae Yoon; CHO, Seongmi; MUN, Jeong Wook; JUNG, Min Woo; LEE, Jung Ha; (29 pag.)US2020/39971; (2020); A1;,
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. 956434-30-3, name is tert-Butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., name: tert-Butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

(step 1) To a solution of (2R)-3-methylbutan-2-ol (0.38 mL) in toluene (8 mL) was added sodium hydride (0.28 g), and the resulting mixture was stirred at 70C for 15 min under a nitrogen atmosphere. A mixture of tert-butyl 8-chloro-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (1.0 g), BINAP (0.066 g), Pd2(dba)3 (0.048 g) and toluene (8 mL) was added, and the resulting mixture was stirred at 100C for 2 hr under an argon atmosphere. The reaction solution was poured into water, and the resulting product was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (solvent gradient; 0?40% ethyl acetate/hexane) to give tert-butyl 8-{[(1R)-1,2-dimethylpropyl]oxy}-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate (0.77 g, 65%) as a white powder. 1H-NMR(CDCl3):delta0.94(3H,d,J=6.8Hz), 0.96(3H,d,J=6.6Hz), 1.23(3H,d,J=6.2Hz), 1.43(9H,s), 1.82-1.95(1H,m), 3.81(2H,brs), 4.21(2H,brs), 4.34-4.43(2H,m), 4.97(1H,brs), 6.40(1H,brs), 7.30-7.50(1H,m)

According to the analysis of related databases, 956434-30-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2213675; (2010); A1;,
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. 141449-85-6, name is tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Formula: C11H20N2O2

A catalyst solution was prepared by mixing tris(dibenzylideneacetone)dipalladium (Pd2(dba)3; 35 mg, 0.038 mmol; Alfa) and racemic 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP; 61 mg, 0.098 mmol; Strem) in toluene (1 mL) and heating the mixture to 80 C. for 15 min. The solution was cooled, and then added to a mixture of 3-Boc-3,7-diazabicyclo[3.3.0]octane (483 mg, 2.28 mmol; see WO 0181347) and 2,7-dibromofluoren-9-one (336 mg, 0.994 mmol; Aldrich) in toluene (5 mL). Sodium tert-butoxide (276 mg, 2.87 mmol; Aldrich) was then added, and the reaction mixture was purged with nitrogen and heated to 80-85 C. overnight (16 h). After cooling to room temperature, the mixture was filtered through diatomaceous earth and purified by chromatography (80 g silica gel, 10-100% EtOAc-hexanes) to afford the title compound (322 mg, 0.537 mmol, 54% yield). MS (DCl/NH3): m/z 601 (M+1)+.

According to the analysis of related databases, 141449-85-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Schrimpf, Michael R.; Sippy, Kevin B.; Ji, Jianguo; Li, Tao; Frost, Jennifer M.; Briggs, Clark A.; Bunnelle, William H.; US2005/234031; (2005); A1;,
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. 98-64-6, name is 4-Chlorobenzenesulfonamide, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 98-64-6

General procedure: The toluene (2 mL) suspension of silica gel (200-300 mesh, 0.1 g), TfOH (7.7 mg, 0.05 mmol) and water (20 muL) was stirred in a test-tube at room temperature for 30 min. Then alkene (2 mmol or 4 mmol) and sulfonamide (1 mmol) were added to the suspension and the reaction mixture was stirred at 70 oC (or 85 oC). The course of the reaction was monitored by TLC. After the completion of the reaction, the mixture was cooled to room temperature and the reactor was centrifuged (2000 r/min) for 2 min and the solution was removed by syringe. The catalyst was then washed with toluene (1 mL) twice with the same procedure and a new reaction was carried out by adding the new batch of alkene (2 mmol), sulfonamide (1 mmol) and toluene (2 mL) to the recovered catalyst. The solution containing the product was purified through a silica gel flash column to afford the product.

According to the analysis of related databases, 98-64-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Pei Nian; Xia, Fei; Zhao, Zheng Le; Wang, Qing Wei; Ren, Yu Jie; Tetrahedron Letters; vol. 52; 46; (2011); p. 6113 – 6117;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 631-58-3, These common heterocyclic compound, 631-58-3, name is Propanethioamide, 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.

A mixture of propanethioamide (69 mg, 0.78 mmol) and (S)-tert-butyl 4-bromo-1-(4-nitrophenyl)-3-oxobutan-2-ylcarbamate, 7, (0.300 g, 0.77 mmol) in CH3CN (4 mL) is refluxed for 2 hours. The reaction mixture is cooledto room temperature and diethyl ether is added to precipitate the intermediate 2-(nitrophenyl)-(S)-1-(4-ethylthiazol-2-yl)ethylamine which is isolated by filtration as the hydrobromide salt. The hydrobromide salt is dissolved in DMF (8 mL)together with diisoproylethylamine (0.38 mL, 2.13 mmol), 1-hydroxybenzotriazole (107 mg, 0.71 mmol) and (S)-(2-methoxycarbonyl-amino)-3-phenylpropionic acid (175 mg, 0.78 mmol). The mixture is stirred at 0 C for 30 minutes thenat room temperature overnight. The reaction mixture is diluted with water and extracted with EtOAc. The combinedorganic phase is washed with 1 N aqueous HCl, 5 % aqueous NaHCO3, water and brine, and dried over Na2SO4. Thesolvent is removed in vacuo to afford 0.300g (81% yield) of the desired product which is used without further purification.LC/MS ESI+MS 483 (M+1).

Statistics shows that Propanethioamide is playing an increasingly important role. we look forward to future research findings about 631-58-3.

Reference:
Patent; Aerpio Therapeutics, Inc.; PETERS, Kevin, G.; SHALWITZ, Robert; (176 pag.)EP2624916; (2018); B1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 2895-21-8,Some common heterocyclic compound, 2895-21-8, name is N-Isopropyl-2-chloroacetamide, molecular formula is C5H10ClNO, 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: The reaction mixture of N-substituted-2-chloroacetamide 2 (5.0 mmol, 1.0 equiv), crude product of 2-bromo-4-(substituted methyl)phenol 7 (5.0mmol, 1.0 equiv) and K2CO3 (7.5 mmol, 1.0 equiv) in MeCN (40 mL) was refluxed and monitored by TLC. When the reaction was accomplished, the solvents were removed under vacuum. To the obtained residue, water (50 mL)was added. The mixture was then extracted by ethyl acetate (3 x 50 mL), and the combined organic layers were dried over MgSO4. Removal the MgSO4 and evaporation of the solvent at reduced pressure gave the crude product. The pure product 8 was obtained by column chromatography on silica gel (elute: ethyl acetate: petroleum = 1: 4).

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

Reference:
Article; Xia, Shuai; Liu, Ji-Qiang; Wang, Xiu-Hua; Tian, Ye; Wang, Yu; Wang, Jing-Huan; Fang, Liang; Zuo, Hua; Bioorganic and Medicinal Chemistry Letters; vol. 24; 6; (2014); p. 1479 – 1483;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 174799-52-1, 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. 174799-52-1, name is tert-Butyl (2-(benzylamino)ethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a mixture of tert-butyl 2-(benzylamino)ethylcarbamate (2.8 g, 11.2 mmol) and 37% aqueous CH2O (1.0 mL, 11.2 mmol) in 1,2-dicholoroethane (35 mL) at RT was added NaHB(AcO)3 (3.7 g, 11.2 mmol). The mixture was stirred (RT, 16 h), diluted with saturated aqueous NaHCO3 (400 ml) and extracted with EA (3*300 ml). The organic layer was dried over MgSO4 and concentrated under reduced pressure to afford tert-butyl 2-(benzyl(methyl)amino)ethylcarbamate (1.38 g, 46.8%). 1H-NMR (CDCl3): delta7.25 (m, 5H, CH), 3.5 (s, 2H, CH2), 3.3 (m, 2H, CH2), 2.48 (m, 2H, CH2), 2.2 (s, 3H, CH3), 1.4 (s, 9H, CH3).

The synthetic route of tert-Butyl (2-(benzylamino)ethyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Milne, Jill C.; Jirousek, Michael R.; Bemis, Jean E.; Smith, Jesse J.; US2010/41748; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

4943-86-6, name is 2-Amino-N-(4-chlorophenyl)benzamide, 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. COA of Formula: C13H11ClN2O

General procedure: A mixture of 4-methoxybenzyl alcohol (0.138 g, 1 mmol), I2 (0.254 g, 1 mmol), K2CO3(0.138 g, 1 mmol), isatoic anhydride (0.163 g, 1 mmol) and aniline (0.093 g,1 mmol) in water (5 mL) was stirred for 3 h at reflux. After reaction completion,the mixture was cooled to room temperature and stirred for 1 h. The resultingprecipitate was filtered, washed with water (3 3 mL), and purified by recrystallization from ethanol to give 4a as a white solid.

The synthetic route of 4943-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Azimi, Seyedeh Bahareh; Azizian, Javad; Tetrahedron Letters; vol. 57; 2; (2016); p. 181 – 184;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics