Tag: M.W=100-200

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

Weigh 6-methoxybenzothiazole (0.5mmol, 83mg), K2S2O8 (2mmol, 0.54g) and Eosin Y (0.01mmol, 6.5mg) in a 25mL Schlenk reaction tube, and then add N, N-dimethyl Propionamide (38mmol, 3.8g) was placed under a 20W power LED white light to react. The reaction was stirred at room temperature. The progress of the reaction was monitored by TLC. The reaction was completed after 24 hours. The reaction solution was concentrated to remove the solvent. Separation (eluent: petroleum ether / ethyl acetate with a volume ratio of 5: 1) gave a yellow oil, namely the derivative Il. Yield: 74%.

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

Reference:
Patent; Zhejiang University of Technology; Weng Jianquan; Xu Wenxiu; Dai Xiaoqiang; Liu Xinghai; (11 pag.)CN110432282; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 37045-73-1, name is 3-(Methylsulfonamido)aniline, 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 37045-73-1, Application In Synthesis of 3-(Methylsulfonamido)aniline

In a 1000 mL four-necked flask with mechanical stirring and a thermometer,Add 700g of water,Methanesulfonamidoaniline 149g(content 80%, 0.64 mol),Calcium carbonate 150g (1.50mol),Stir well and then as solution A,Transfered to the pipeline reactor by screw pump A,At the same time pumping liquid 1-chlorohexane 163g (1.35mol),Solution A and 1-chlorohexane are fed with screw pump A and screw pump B, respectively.The mass flow rate ratio of the control solution A to 1-chlorohexane was 6.1:1.0.The pipeline reactor has a pipeline reaction section providing a chemical reaction site, and the solution A and 1-chlorohexane are continuously reacted in the pipeline reaction section.Keep the temperature of the pipeline reaction section at 135 C,Control the residence time of the reaction solution to 10 min,Cooled, extracted with 800 mL of 2-methyltetrahydrofuran.The combined organic phases are concentrated under reduced pressure.Obtaining dialkylaminomethanesulfonanilide214.1g,97.6%,The yield was 94.5%.

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, 3-(Methylsulfonamido)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JIANGSU DIAN CHEMICAL CO LTD; Jiangsu Di’an Chemical Co., Ltd.; ZHEJIANG SHANYU TECH CO LTD; Zhejiang Shanyu Technology Co., Ltd.; TAO ANNI; Tao Anni; GUO HAIBIN; Guo Haibin; WEI BIN; Wei Bin; LI JIAN; Li Jian; ZHENG TUCAI; Zheng Tucai; XU XUMING; Xu Xuming; HU XIAOKUI; Hu Xiaokui; (6 pag.)CN108299250; (2018); A;,
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These common heterocyclic compound, 156731-40-7, name is 1-(Boc-amino)-3-butene, 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. Quality Control of 1-(Boc-amino)-3-butene

Intermediate 154. tert-butyl but-3-en-1 -yl(methyl)carbamate To a 0 C solution of tert-butyl but-3-en-1 -ylcarbamate (Intermediate 62, 840mg, 4.9mmol) in THF (20ml_) was added, under inert atmosphere, sodium hydride (216mg of a 60% dispersion in oil, 8.99mmol) and the reaction mixture was stirred at r.t. for 1 h before methyl iodide (3.05ml_, 49.0mmol) was added. The reaction mixture was heated to reflux and maintained at this temperature overnight. Ice was then added and the aquous phase was extracted with ethyl acetate (3 x 50ml_). The combined organic extracts were washed with brine, filtered and concentrated to dryness to afford the title compound as a colorless oil (893mg, 98%). 1 H NMR (300 MHz, cdcl3) delta 5.75 (dddd, J = 17.1 , 13.7, 6.8, 3.4 Hz, 1 H), 5.17 – 4.92 (m, 2H), 3.39 – 3.08 (m, 2H), 2.84 (s, 3H), 2.37 – 2.13 (m, 2H), 1 .45 (s, 9H).

The synthetic route of 1-(Boc-amino)-3-butene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALMIRALL, S.A.; PUIG DURAN, Carlos; AIGUADE BOSCH, Jose; GUAL ROIG, Silvia; PRAT QUINONES, Maria; (149 pag.)WO2016/46390; (2016); A1;,
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Reference of 360-64-5, The chemical industry reduces the impact on the environment during synthesis 360-64-5, name is 2-(Trifluoromethyl)benzamide, I believe this compound will play a more active role in future production and life.

Methyl S-chloropyrazine-2-carboxylate (879 mg), 2-trifluoromethylbenzamide (1.OS g), Cs2CO3 (2.31 g), xantphos (0.268 g), and Pd2(dba)3 (0.141 g) were stirred in dioxane (25.5 mL) under argon atmosphere at 80C for 6 hours. The mixture was cooled, and then AcOEt and water were added thereto and the mixture was stirred. Then, insoluble substances were filtered through Celite. The filtrate was separated, and the organic layer was washed with water and saturated brine, dried over anhydrous Na2 SO4, and filtered. The solvent was removed, and then the resulted residue was purified by column chromatography (Hexane/AcOEt). The resultant was confirmed as methyl S-[(2-(trifluoromethyl)benzamidojpyrazine-2-carboxylate (1.69 g) by 1H-NMR (CDC13MeOH (16.5 mL) was added thereto, and then thereto was added SN aqueous NaOH solution (4.1 mL) under ice cooling. The mixture was stirred at room temperature for 4 hours. The mixture was adjusted to pH=4 by addition of 5N HC1 (4.1 mL) and the resulted precipitate was filtered and dried at 60C to give5- [2-(trifluoromethyl)benzamidojpyrazine-2-carboxylic acid (1.56 g).

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-(Trifluoromethyl)benzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; KAN, Keizo; TAKUWA, Masatoshi; TANAKA, Hirotaka; FUJIWARA, Hideto; YAMABE, Hokuto; MATSUDA, Satoshi; OHDACHI, Kazuhiro; HANARI, Taiki; MENJO, Yasuhiro; URUSHIMA, Tatsuya; FUJITA, Shigekazu; (183 pag.)WO2019/4421; (2019); A1;,
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Synthetic Route of 2675-89-0, 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. 2675-89-0, name is 2-Chloro-N,N-dimethylacetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a suspension of (4aR,4bS,6aS,9aS,9bR)-4a,6a-dimethyl-4,4a,4b,5,6,6a,9,9a,9b,10-decahydro-1H-indeno[5,4-f]quinoline-2,7(3H,8H)-dione (794 mg, 2.7 mmol) in anhydrous DMF (30 mL) was added NaH (60%, 324 mg, 8.1 mmol) and 2-chloro-N,N-dimethylacetamide (670 mg, 5.5 mmol) at 0 C., then the reaction was stirred under 50 C. for 2 hour. Then cooled down to room temperature and partitioned between ethyl acetate (20 mL) and water (20 mL). The layers were separated and the aqueous layer extracted with ethyl acetate (25 mL¡Á3). The combined organic layers were dried over Na2 SO4. After filtration, the organic phase was concentrated under vacuum to afford 2-((4aR,4bS,6aS,9aS,9bR)-4a,6a-dimethyl-2,7-dioxo-2,3,4,4a,4b,5,6,6a,7,8,9,9a,9b,10-tetradecahydroindeno[5,4-f]quinolin-1-yl)-N,N-dimethylacetamide as a yellow solid (760 mg, yield 74%). 1H-NMR (400 MHz, CDCl3): 4.82 (m, 1H), 4.15 (m, 1H), 3.06 (s, 3H), 2.97 (m, 3H), 2.50 (m, 3H), 2.25 (m, 1H), 2.14 (m, 1H), 1.19 (m, 12H), 1.15 (s, 3H), 0.90 (s, 3H). LC-MS (m/z) 373 [M+H]+.

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

Reference:
Patent; LEAD THERAPEUTICS, INC.; US2010/105700; (2010); A1;,
Amide – Wikipedia,
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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. 5202-85-7, name is 2-Amino-5-chlorobenzamide, A new synthetic method of this compound is introduced below., Safety of 2-Amino-5-chlorobenzamide

General procedure: A 12mL vial was charged with MCM-41-2P-Pd(OAc)2 (2mol%), 2-aminobenzamide (1mmol), aryl iodide (1mmol) (if solid) and a stirring bar. Then, DMF (2mL), aryl iodide (1mmol) (if liquid) and DBU (2mmol) were injected by syringe under an argon atmosphere. The vial was placed in an alloy plate, which was transferred into a 300mL Parr Instruments 4560 series autoclave under an argon atmosphere. After flushing the autoclave three times with CO, a pressure of 10bar CO was fixed at ambient temperature. The autoclave was heated for 20hat 120C. After completion of the reaction, the autoclave was cooled to room temperature and the pressure was released carefully. The reaction mixture was diluted with ethyl acetate (10mL) and filtered. The palladium catalyst was washed with distilled water (2¡Á5mL) and acetone (2¡Á5mL), and reused in the next run. The filtrate was concentrated in vacuo and the pure product was isolated by either washed with water, ethyl acetate and finally hexane or recrystallization from MeOH.

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; You, Shengyong; Huang, Bin; Yan, Tao; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 875; (2018); p. 35 – 45;,
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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. 78191-00-1, name is N-Methoxy-N-methylacetamide, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C4H9NO2

Intermediate 8: To a solution of 5-methylthiazole (0.179 mL, 2.017 mmol) in ether (13.63 mL) was added nBuLi (1.387 mL, 2.219 mmol, 1.6 M in hexanes) dropwise at -78 C and the reaction mixture was stirred at this temperature for 15 mm. A solution of N-methoxy-N-methylacetamide (229 mg, 2.2 19 mmol) in THF (4.0 mL) was addeddropwise and the reaction mixture warmed to rt and stirred for 1 h. The reaction mixture was quenched with sat. NH4C1. The organic layer was separated and washed with water, brine, dried over anhydrous Na2SO4, filtered and concentrated. The crude product was purified by chromatography to yield Intermediate 8 (123 mg, 0.87 1 mmol, 43.2% yield) as a pale yellow solid. ?H NMR (500 MHz, CDC13) oe 7.66 (s, 1H), 2.68 (s, 3H), 2.57 (s,3H). LCMS Anal. Calc?d for C6H7NOS 141.0, found [M+H] 141.9.

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 78191-00-1.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; MENG, Wei; ZHAO, Guohua; WO2015/134701; (2015); 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. 16066-84-5, name is tert-Butyl methylcarbamate, A new synthetic method of this compound is introduced below., Product Details of 16066-84-5

Description 84; 1,1-Dimethylethyl (6-formyl-3-pyridinyl)methylcarbamate (D84); A mixture of 5-bromo-2-pyridinecarbaldehyde (1.5 g, 8.064 mmol), 1 ,1-dimethylethyl methylcarbamate (D83) (1.267 g, 9.677 mmol), tris(dibenzylideneacetone) dipalladium(O) (0.148 g, 0.161mmol), xantphos (0,373 g, 0.645 mmol) and cesium carbonate (3.678 g, 11.289 mmol) in dioxane (35 mL) was heated at 11O0C overnight under an argon atmosphere. On cooling, the solvent was removed in vacuo and the residue partitioned between EtOAc and water. The organic layer was separated, washed with water and brine, dried and concentrated to give the crude product which was purified by column chromatography. Elution with 0-50% ether/petroleum ether gave the title compound as a brown oil (0.977 g). deltaH (CDCI3, 400MHz) 10.01 (1 H, s), 8.79 (1 H, d), 7.94 (1 H, d), 7.86 (1 H, dd), 3.40 (3H, s), 1.53 (9H, s). MS (ES+): 259.1 (MNa+), 181.2, no molecular ion (MH+) observed.

The synthetic route of 16066-84-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/729; (2008); A1;,
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Adding a certain compound to certain chemical reactions, such as: 147751-16-4, name is tert-Butyl methylsulfonylcarbamate, 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 147751-16-4, Recommanded Product: tert-Butyl methylsulfonylcarbamate

N-{l-[(lS,3R)-3-(2,2,2-Trifluoro-ethylamino)-cyclopentyl]-lH-imidazo[4,5-c]quinolin-2- ylmethyl} -methanesulfonamideN-tert-Butylcarbamate-N-{l-[(lS,3R)-3-(2,2,2-trifluoro-ethylamino)-cyclopentyl]-lH- imidazo[4,5-c]quinolin-2-ylmethyl} -methanesulfonamide A suspension of {l-[(lS,3R)-3-(2,2,2-trifluoro-ethylamino)-cyclopentyl]-lH-imidazo[4,5- c]quinolin-2-yl} -methanol (139 mg, 0.38 mmol) in anhydrous THF (3.8 mL), under an atmosphere of nitrogen was treated with tert-butyl N-methanesulfonylcarbamate (164 mg, 0.84 mmol), followed by triphenylphosphine (200 mg, 0.76 mmol) and then diisopropyl azodicarboxylate (150 mu?, 0.76 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was diluted with EtOAc and water and the phases separated. The aqueous layer was extracted with EtOAc (2x) and the combined organic phases washed (brine), dried (sodium sulfate) and concentrated in vacuo to afford 780 mg of a yellow oil. Purification by column chromatography on an Isolute SCX-2 cartridge (eluting with MeOH and then 2M NH3 in MeOH) afforded 192 mg of a golden glassy solid. This was purified by filtration through a pad of silica gel (gradient: 0 to 2% [2M NH3 in MeOH] in EtOAc) to afford 169 mg (82%) of N-tert-butylcarbamate-N- { 1 – [( 1 S ,3R)-3 -(2,2,2-trifluoro-ethylamino)-cyclopentyl] – 1 H- imidazo[4,5-c]quinolin-2-ylmethyl}-methanesulfonamide as a colourless gum. LCMS (Method B, ESI): RT = 2.67 min, m+H = 542.0; 1H NMR (400 MHz, CDC13): delta 9.20 (s, 1 H), 8.40 (d, 1 H), 8.28 (d, 1 H), 7.66 (m, 2 H), 5.54-5.30 (m, 3 H), 3.68 (s, 3 H), 3.60 (m, 1 H), 3.30 (m, 2 H), 2.60 (m, 2 H), 2.33 (m, 1 H), 2.15 (m, 2 H), 1.98 (m, 1 H), 1.50 (s, 9 H).

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:
Patent; F. HOFFMANN-LA ROCHE AG; HURLEY, Christopher; KULAGOWSKI, Janusz; ZAK, Mark; WO2013/7768; (2013); 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. 683-57-8, name is 2-Bromoacetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 683-57-8

INTERMEDIATE 226: methyl 3-(2-amino-2-oxoethoxy)-5-(5-((((R)-2-((R)-1-(N- (benzyloxy)formamido) propyl)heptanamido)methyl)carbamoyl)furan-2-yl)benzoate A mixture of methyl 3-(5-((((R)-2-((R)-1-(N- (benzyloxy)formamido) propyl) heptanamido) methyl)carbamoyl)furan-2-yl)-5-hydroxybenzoate (0.25 g, 0.42 mmol), 2-bromoacetamide (0.116 g, 0.842 mmol), and K2003 (0.29 g, 2.106 mmol) in acetonitrile (1.50 ml) was heated at 8000 for 1 hour. The reaction was then cooled to RT and concentrated in-vacuo. The residue was partitionedbetween H20 and EtOAc and the organic layer was separated. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated under vacuum to afford a white solid. The solid was purified by flash column chromotography (20- 100%EtOAc:Hexane) to afford the titled compound.(0.22 g, 80 % yield) as white solid. MS (mlz) 651.2 (M+H+).

The synthetic route of 683-57-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; DOWDELL, Sarah E.; EIDAM, Hilary Schenck; ELBAN, Mark; FOX, Ryan Michael; HAMMOND, Marlys; HILFIKER, Mark A.; HOANG, Tram H.; KALLANDER, Lara S.; LAWHORN, Brian Griffin; MANNS, Sharada; PHILP, Joanne; WASHBURN, David G.; YE, Guosen; WO2015/104684; (2015); A1;,
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