Author: Jessica.F

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. 22227-26-5, name is 3,5-Bis(trifluoromethyl)benzamide, A new synthetic method of this compound is introduced below., SDS of cas: 22227-26-5

Charged 3,5-bis(trifluoromethyl)benzonitrile (100 gm, 1 meq.), 2 (N) Sodium hydroxide (21.7 gm, 1.3 meq.) into 400 ml methanol and stirred the reaction mass at 20 – 30¡ãC for 2-3 hrs. Added Dimethyl sulphoxide (100 ml) followed by dilute 30percent H202 solution (100 gm diluted in 300m1 water, 2.1 eq.) at 20 -35¡ãC. Stirred the mass for 2-3 hrs. at 20-30¡ãC and confirmed reaction completion by HPLC. Reaction mass quenched by addition of water (500 ml, S Vol). Filtered the slurry and washed the wet cake by water (500 ml, SVol). Dried under vacuum at 50-60¡ãC to get 100 gm 3, 5-bis (trifluoromethyl) benzamide (Purity 99 percent). Charged 3, 5-bis (trifluoromethyl) benzamide, prepared according to procedures a or b, as described above, (100 gm, 1 meq) into N, N Dimethyl formamide (100 ml, 1 vol). Added N, N Dimethyl formamide dimethyl acetal (70 gm, 1.5 meq) at 20-30¡ãC and stirred the reaction mass for 2-3 hrs. Reaction completion for the formation N-((dimethylamino)methylene)-3,5- bis(trifluoromethyl)benzamide was confirmed by HPLC. Cooled reaction mass to 10-15¡ãC and added acetic acid (S00 ml, S vol.) followed by hydrazine hydrate (31 gm, 1.5 meq). Reaction mass was heated to S0-SS¡ãC and stirred for 2-3 hrs. at same temparature. Reaction was monitored by HPLC. Cooled reaction mass to 20-30¡ãC and quenched by addition of water (2.S L, 2S vol.). Filtered the slurry and washed the wet cake by water (S00 ml, S vol.). Dried under vacuum at 50-60¡ãC to get 3 -(3,5 -bis(trifluoromethyl)phenyl)- 1 H-i ,2,4-triazole (94 gr, Purity 97percent).

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; WATSON LABORATORIES INC.; MUTHUSAMY, Anantha Rajmohan; KANNIAH, Sundara Lakshmi; RAVI, Akash; DAS, Tonmoy Chitta; CHEMATE, Rajendra Popat; SINGH, Anil Kumar; WAGH, Yogesh Dhananjay; (60 pag.)WO2018/129227; (2018); A1;,
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These common heterocyclic compound, 147751-16-4, name is tert-Butyl methylsulfonylcarbamate, 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 tert-Butyl methylsulfonylcarbamate

To a solution of benzyl 4-(hydroxymethyl)-3,3-dimethyl-pyrrolidine-1-carboxylate (300 mg, 1.14 mmol), tert-butyl N-methylsulfonylcarbamate (330 mg, 1.7 mmol) and PPh3 (890 mg, 3.4 mmol) in THF (20 mL) was added DEAD (390 muL, 2.5 mmol) dropwise and the reaction mixture stirred at ambient temperature under N2 for 16 hours. The reaction mixture was concentrated in vacuo and the residue purified by column chromatography (silica, 0 to 50% EtOAc/PE gradient elution) to give benzyl 4-[[tert- butoxycarbonyl(methylsulfonyl)amino]methyl]-3,3-dimethyl-pyrrolidine-1-carboxylate as a colourless oil that was taken directly on to the next step; MS m/z: 441 (M+H)+.

The synthetic route of tert-Butyl methylsulfonylcarbamate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK PATENT GMBH; VERTEX PHARMACEUTICALS INCORPORATED; BAYLY, Andrew; BLEICH, Matthew; CHARRIER, Jean-Damien; DODD, James; DURRANT, Steven; ENO, Meredith Suzanne; ETXEBARRIA I JARDI, Gorka; EVERITT, Simon; FRAYSSE, Damien; KELLY, Shazia; KNEGTEL, Ronald; MOCHALKIN, Igor; MORTIMORE, Michael; NORTH, Kiri; PORICHIS, Filippos; PULLIN, Robert; RUTHERFORD, Alistair; STORCK, Pierre-Henri; TWIN, Heather Clare; XIAO, Yufang; (1159 pag.)WO2019/148132; (2019); A1;,
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Electric Literature of 78191-00-1,Some common heterocyclic compound, 78191-00-1, name is N-Methoxy-N-methylacetamide, molecular formula is C4H9NO2, 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 STIRRED solution of n-BuLi (2M in pentane ; 15.24 mL, 0.0305 mol) in 70 mL of dry ether at-78C was added dropwise 29 (6.3 g, 0.0277 mol) in 30 mL of ether over a period of 30 minutes. The mixture was stirred for lh, then N-methoxy-N-methylacetamide (3.83 mL, 0.036 mol) was added dropwise over 10 minutes. After lh of stirring at-78C the reaction mixture was washed with sat’d NAHCO3 and extracted with ether. The organic layer was dried with NA2S04 and concentrated in vacuo to give 6.66 g (89%) of 16 as an oil that was used directly for the next step.

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

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WO2004/87699; (2004); A2;,
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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. 37073-15-7, name is 1-(Methylsulfonyl)-1H-benzo[d][1,2,3]triazole, A new synthetic method of this compound is introduced below., Product Details of 37073-15-7

General procedure: A mixture of alpha,beta-unsaturated aromatic or aliphatic acid (10 mmol), CH3SO2Bt (10 mmol) and Et3N (15 mmol) were refluxed in dry THF (50 mL) overnight. The solvent was evaporated and the residue was dissolved in CH2Cl2 (100 mL). The organic phase was washed with brine (3 times) and dried over anhydrous Na2SO4. The organic phase was concentrated under vacuum to give a crude product, which could be further purified by recrystallization from a proper solvent.

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; Xia, Ziming; Lv, Xin; Wang, Wencun; Wang, Xiaoxia; Tetrahedron Letters; vol. 52; 38; (2011); p. 4906 – 4910;,
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Reference of 61903-11-5, These common heterocyclic compound, 61903-11-5, name is 1-(1,4-Diazepan-1-yl)ethanone, 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.

Lithium aluminum hydride (38.2 ml, 38.19 mmol) was added to 1-(1,4-diazepan-1-yl)ethanone (1.697 g, 11.93 mmol) in THF (59.7 ml) at 0 C. under nitrogen. The resulting solution was stirred at ambient temperature for 1 h and then at 60 C. for 1 h. The cooled reaction mixture was poured onto ice (500 mL), acidified with HCl (2M aqueous solution) and purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH and evaporated to dryness to afford 1-ethyl-1,4-diazepane (0.610 g, 40%) as a yellow liquid. This was used directly with no further purification. 1H NMR (399.9 MHz, CDCl3) delta 1.07 (3H, t), 1.74-1.80 (2H, m), 2.58 (2H, q), 2.64-2.70 (4H, m), 2.89-2.95 (4H, m).

Statistics shows that 1-(1,4-Diazepan-1-yl)ethanone is playing an increasingly important role. we look forward to future research findings about 61903-11-5.

Reference:
Patent; ASTRAZENECA AB; US2008/153812; (2008); 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. 78191-00-1, name is N-Methoxy-N-methylacetamide, A new synthetic method of this compound is introduced below., Quality Control of N-Methoxy-N-methylacetamide

To 2,7-dibromonaphthalene (1 g, 3.50 mmol) in anhydrous tetrahydrofuran (18 mL), at -78 C. and under an atmosphere of nitrogen, was added a solution of n-butyllithium (2.5 M in hexanes, 1.5 mL, 3.67 mmol) dropwise. The reaction was stirred at -78 C. for 20 min after which N-methoxy-N-methylacetamide (409 muL, 3.85 mmol) was added. After 15 min, the reaction was warmed to RT and stirred for 30 min. The reaction was quenched with 2 M hydrochloric acid and extracted twice with dichloromethane. The combined organic layers were dried through a hydrophobic frit and concentrated in vacuo. The product was purified by silica flash chromatography (iso-hexanes/ethyl acetate, 7/1) to afford the title compound (650 mg, 75%) as a colorless solid.

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; Gilead Sciences, Inc.; Selcia Limited; Aciro, Caroline; Dean, David Kenneth; Dunbar, Neil Andrew; Highton, Adrian John; Jansa, Petr; Karki, Kapil Kumar; Keats, Andrew John; Lazarides, Linos; Mackman, Richard L.; Pettit, Simon N.; Poullennec, Karine G.; Schrier, Adam James; Siegel, Dustin; Steadman, Victoria Alexandra; (169 pag.)US2017/190737; (2017); A1;,
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Application of 16375-88-5, 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. 16375-88-5, name is N-(4-(Hydroxymethyl)phenyl)acetamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A. (4-Acetamido)-phenylmethyl-4-nitrophenylcarbonate To a solution of 242.8 mg of p-nitrophenyl chloroformate in 5 mL of acetonitrile at 0 C. was added sequentially, 165.2 mg of 4-acetamidobenzyl alcohol and 0.13 mL of 4-methyl morpholine. The mixture was stirred for 24 hours and concentrated in vacuo. The residue was taken up in CH2 Cl2 and washed with 5% sodium bicarbonate and brine, dried over magnesium sulfate, filtered and concentrated in vacuo to yield 320 mg of the title compound. TLC: Rf=0.23, 50% EtOAc/hexane.

The synthetic route of N-(4-(Hydroxymethyl)phenyl)acetamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vertex Pharmaceuticals, Incorporated; US5783701; (1998); A;,
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These common heterocyclic compound, 618-48-4, name is 3-Chlorobenzamide, 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. Recommanded Product: 618-48-4

Then slowly raise the temperature, turn on the ultrasonic generator at the same time, control the ultrasonic frequency of 20KHz, the concentrated ultrasonic horn is directly immersed in the reaction liquid of the kettle body, and a large amount of energy is directly transmitted to the reaction medium.Effectively convert electrical energy into ultrasonic energy, and control the size of ultrasonic energy by changing the amplitude of the generator. Use a constant temperature system to make the material react at a constant temperature of 230 ~ 250 C for 2h, and then continue to increase the temperature, control the temperature of 250 ~ 270 C, and react for 2h. To generate a mixture containing m-chlorobenzonitrile, turn off the ultrasonic generator.Crude nitrile was distilled off from the mixture containing m-chlorobenzonitrile under reduced pressure, and the residue after distillation contained intermediate products (ammonium m-chlorobenzoate and m-chlorobenzamide) produced by the reaction, which were left in the ultrasonic thermostat and continued at the next feeding reaction.The crude nitrile is washed with water, filtered, dried and then distilled under reduced pressure to obtain the finished product. The content of m-chlorobenzonitrile measured by high performance liquid chromatography was 97.0%. Calculate the yield. Based on m-chlorobenzoic acid, the yield of finished m-chlorobenzonitrile is 92.5%.The wastewater produced by washing the crude nitrile with water contains available raw materials m-chlorobenzoic acid, the intermediate products ammonium m-chlorobenzoate, and m-chlorobenzamide. The water is recovered by distillation and concentration, and the intermediate products are recovered. After drying, During the secondary reaction, it was put into the reaction kettle as part of the raw materials to continue the reaction.

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

Reference:
Patent; Sanmenxia Huanyu Biochemical Technology Co., Ltd.; Duan Jingjie; Zhang Weimin; Liang Zhenxian; Wei Zhanyong; Tan Jing; Zhang Kun; Wang Xinyue; Wang Yan; Wang Zhiquan; (7 pag.)CN110467541; (2019); A;,
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Electric Literature of 5202-85-7, A common heterocyclic compound, 5202-85-7, name is 2-Amino-5-chlorobenzamide, molecular formula is C7H7ClN2O, 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.

An aromatic amine 1q-1 (0.20 mmol) and a platensimycin acid (0.10 mmol) were weighed.2-(7-Azobenzotriazole)-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HATU) (0.30 mmol) was added to the reaction flask and 1.0 ml was added.N,N-dimethylformamide, stirring at room temperature; slowly adding triethylamine (0.45 mmol), stirring for 12 hours, rotary evaporationSolvent to obtain a crude product, which is subjected to column chromatography to obtain a platensimycin analog2q-1, yield 46%.

The synthetic route of 5202-85-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Changsha Tianci Bio-pharmaceutical Technology Co., Ltd.; Changsha Cihang Pharmaceutical Institute Co., Ltd.; Ha Yao Cihang Pharmaceutical Co., Ltd.; Duan Yanwen; Shen Ben; Huang Yong; Zhu Xiangcheng; Qiu Lin; Tian Kai; (39 pag.)CN107793388; (2018); A;,
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Reference of 5004-88-6, These common heterocyclic compound, 5004-88-6, name is 2-Amino-4,5-dimethoxybenzamide, 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.

To a stirred mixture of 4 g of 2-amino-4,5-dimethoxybenzamide and 200 ml of ether was added dropwise, e solution of 3.3 g of benzoyl isothiocyanate in 100 ml of ether over 15 minutes. After 24 hours, the solid was collected, giving 7 g of the desired product as white crystals, mp 204-207 C. (dec.).

Statistics shows that 2-Amino-4,5-dimethoxybenzamide is playing an increasingly important role. we look forward to future research findings about 5004-88-6.

Reference:
Patent; American Cyanamid Company; US5001157; (1991); A;,
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