Tag: M.W=0-100

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. 33279-01-5, name is 3-Oxopentanenitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 33279-01-5

Weighing 0.22 muM of sodium cyanide (2.2 equiv) in 250 ml three-neck bottle in, under ice bath by adding 110 ml THF, then adding 0.1 muM 1 a (1 equiv) and 0.1 muM 1 d (1 equiv), 65 C reflow 12 h. After the reaction is completed, the right amount of water under ice bath quenching reaction, adjusting solution PH value to 4 – 5, ethyl acetate extraction, the organic phase is dried with anhydrous sodium sulfate, and steaming and get products 2 ad. 250 Ml three-neck bottle is added to the product of the 1st step 2 ad, 100 ml ethanol and 0.9 muM 2 e, 85 C reflow 18 h. Stopping the reaction, steaming and out ethanol, saturated sodium hydroxide solution to adjust the residue for the PH in 9 – 10. DCM extraction, the organic phase is dried with anhydrous sodium sulfate, and steaming and, column chromatography purification (dichloromethane: ethyl acetate=20:1) to obtain the product B4.

The synthetic route of 33279-01-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Agricultural University; Hou Shicong; Gao Gui; Chen Xiangzhu; Liu Jingjing; Zhang Yuanyuan; Zhang Xueyan; (10 pag.)CN107980784; (2018); A;,
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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. 6330-25-2, name is 2-Cyano-N-methyl-acetamide belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2-Cyano-N-methyl-acetamide

After 32.03 parts of phthalonitrile were added to 224.21 parts of formamide and stirred, 39.0 parts of sodium hydroxide was added and the mixture was stirred at 50 C. for 1 hour.320 parts of water and 25.75 parts of 2-cyano-N-methylacetamide were added, and the mixture was stirred at 50 C. for 2 hours. Next, 640 parts of 80% acetic acid and 36.82 parts of barbituric acid were added, and the mixture was stirred at 90 C. for 3 hours. After cooling to 80 C., the non-volatile components were filtered off with a Buchner funnel and washed with 3000 parts of water.

The synthetic route of 6330-25-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Toyo Ink Mfg. Co., Ltd.; Aikyo, Sumihiro; Nishida, Kazufumi; (40 pag.)JP2020/26503; (2020); A;,
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Application of 630-18-2,Some common heterocyclic compound, 630-18-2, name is Pivalonitrile, molecular formula is C5H9N, 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.

5) Example 1-5:Preparation of methyl trimethylacetimidate hydrochlorideTo a reactor were added 1.6 kg of trimethylacetonitrile and 1.48 kg of methanol andthe reactor was cooled to -10C. Acety 1 chloride in the amount of 1. 81 kg was slow 1 yadded thereto and the mixture was stirred at 0Cfor 12 hours. While stirring, theinternal temperature of the reactor was maintained at ooc. Upon termination of thereaction, the solvent was removed at 45C under reduced pressure. To the reactionmixture was added 11.8 kg of tert-butyl methyl ether and the mixture was stirred at oocfor 3 hours. The resulting solid was filtered and vacuum-dried at 40C to obtain 2.63kg of methyl trimethylacetimidate hydrochloride (yield: 90% ).1H-NMR (400MHz, DMSO-d6): 11.7(s, 2H), 4.07(s, 3H), l.O(s, 9H)

The synthetic route of 630-18-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CJ HEALTHCARE CORPORATION; KWEON, Jae Hong; KIM, Eun Sun; SONG, Seog Beom; LEE, Sung Ah; LEE, Ji Yun; CHOI, Kwang Do; PARK, Young Joon; WO2015/5615; (2015); A1;,
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Synthetic Route of 33279-01-5, The chemical industry reduces the impact on the environment during synthesis 33279-01-5, name is 3-Oxopentanenitrile, I believe this compound will play a more active role in future production and life.

Example 57A; 5-ethyl-[ 1 ,2,4]triazolo[ 1 ,5-a]pyrimidin-7-amineA mixture of 3-oxopentanenitrile (1.0 g, 10.3 mmol) and 3-amino-l,2,4-triazole (0.91 g, 10.8 mmol) in 10 mL of acetic acid was heated in a pressure tube at 150 0C for 24h. The reaction mixture was allowed to cool to room temperature, and solvent was removed in vacuo. The solid was removed via filtration. The filtrate partially solidified upon standing at room temperature, and the solid was collected via filtration to give the title compound (200 mg, 12% yield).

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

Reference:
Patent; ABBOTT LABORATORIES; WO2008/134690; (2008); 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 4426-11-3 as follows. Safety of Cyclobutanecarbonitrile

Example 275B 1-(1-methyl-1H-benzo[d]imidazol-2-yl)cyclobutanecarbonitrile To a solution of Example 275A (1.90 g, 11.4 mmol) in toluene (30 mL) was added cyclobutanecarbonitrile (1.01 g, 12.5 mmol) and potassium hexamethyldisilazide (34.2 mL, 17.1 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was poured into 1N HCl solution (50 mL) and the aqueous layer was extracted with EtOAc (3*20 mL). The combined layers were washed with brine (100 mL), dried over MgSO4, filtered, and concentrated. The residue was purified by prep. TLC on silicagel (eluted with EtOAc: petroleum ether=1:10) to give the title compound (1.0 g, 4.69 mmol, 41.1% yield) as a white solid. MS: MS (M+H)+; 1H NMR (400 MHz, CDCl3): delta 7.80-7.78 (m, 1H), 7.36-7.30 (m, 3H), 3.83 (s, 3H), 3.13-3.05 (m, 2H), 2.99-2.92 (m, 2H), 2.48-2.41 (m, 1H), 2.24-2.18 (m, 1H).

According to the analysis of related databases, 4426-11-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; AbbVie Inc.; Bayburt, Erol K.; Clapham, Bruce; Cox, Phil B.; Daanen, Jerome F.; Dart, Michael J.; Gfesser, Gregory A.; Gomtsyan, Arthur; Kort, Michael E.; Kym, Philip R.; Schmidt, Robert G.; Voight, Eric A.; US2013/131036; (2013); A1;,
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Synthetic Route of 2469-99-0,Some common heterocyclic compound, 2469-99-0, name is 3-Oxobutanenitrile, molecular formula is C4H5NO, 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 stirring suspension of 4-hydrazinylisoqui- noline (0.32 g, 2.0 mmol) and 3-oxo-butyronitrile (0.16 g, 0.19 mmol) in ethanol (10 mE) was heated at 80 C. for 3 h. After cooling to room temperature, 20% aqueous sodium hydroxide (1 mE) was added to the reaction mixture and was further heated at 80 C. for 1 h. The reaction mixture was cooled to room temperature and concentrated in vacuo. The crude residue was dissolved in 1: 1 dichloromethane/methanol (40 mE) and the phases were separated. The organic layer was dried (Na2SO4), and filtered through a pad of Celite. The filtrate was concentrated in vacuo and the crude residue was purified by flash chromatography (Si02, 50-100% ethyl acetate in hexanes) to give the desired product (0.36 g, 1.6 mmol, 81%)

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

Reference:
Patent; ChemoCentryx, Inc.; Cappel, Markus; (83 pag.)US2018/9797; (2018); A1;,
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Electric Literature of 98730-77-9,Some common heterocyclic compound, 98730-77-9, name is 1-(Hydroxymethyl)cyclopropanecarbonitrile, molecular formula is C5H7NO, 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.

PPh3 (6.48 g, 24.71 mmol) and imidazole (1.682 g, 24.71 mmol) were dissolved in DCM (35 ml) and stirred at 0C. After 5 minutes, iodine (5.75 g, 22.65 mmol) was added. The resulting suspension was stirred at the same temperature for another 30 min. The solution of 1- (hydroxymethyl)cyclopropanecarbonitrile (2 g, 20.59 mmol) in 2 ml of DCM was added to the reaction mixture. The resulting mixture was then stirred at RT for 2 h, after which it was diluted with 20 ml water and 30 ml of satd. Na2S2O3 solution. About 50 ml of ether was added to the flask. The organics were extracted twice using 50 ml of ether, separated and dried over anhydrous MgSO4. The solids were filtered out, and the filtrate was carefully concentrated in vacuo and then directly loaded on a silica gel column and eluted with 0-30% EtOAc in hexanes to afford the title compound.1H NMR (CDCl3, 5000+]^^^^3.18 (s, 2H), 1.16-1.20 (m, 2H), 0.99-1.08 (m, 2H).

The synthetic route of 98730-77-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; SHEN, Dong-Ming; KUANG, Rongze; KUMAR, Puneet; DUFFY, Joseph, L.; ZHU, Cheng; ALI, Amjad; YANG, Meng; DEBENHAM, John, S.; (124 pag.)WO2018/39094; (2018); A1;,
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6011-14-9, name is 2-Aminoacetonitrile hydrochloride, belongs to nitriles-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. Recommanded Product: 6011-14-9

2-trifluoromethylpyridine-5-carboxylic acid (0.191 g, 1.0 mmol)And aminoacetonitrile hydrochloride (0.081 g, 1.0 mmol)Dissolved in 25 mL of dichloromethane,Add triethylamine (0.202 g, 2.0 mmol),Then EDC (0.287 mg, 1.5 mmol) was added.HOBt (0.20g, 1.5mmol),Reaction at 25 C for 3 h,After TLC detects the reaction,The reaction solution was first washed with water (20 mL*2).Wash with saturated brine (20ml*1),After drying with anhydrous sodium sulfate,Desolvent, get crude,The crude product was purified by column chromatography to give a white solid.M.p. 83-85 C, yield: 88%.

The synthetic route of 6011-14-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Kaiai Network Technology Co., Ltd.; Xu Liyong; (6 pag.)CN108623518; (2018); A;,
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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. 4426-11-3, name is Cyclobutanecarbonitrile, This compound has unique chemical properties. The synthetic route is as follows., Safety of Cyclobutanecarbonitrile

A solution of borane in THF (1M, 296 mL, 296 mmol) was added to a solution of cyclobutanecarbonitrile (20 g, 247 mmol) in THI (60 niL) under argon, and the mixture heated under reflux overnight. The mixture was cooled in an ice-water bath and MeOH (120 niL) added dropwise while keeping the temperature of the mixture below 20 C. HCI inMeOH (4M, 300 mL) was added, againkeeping the temperature below 20 C. The resulting solutionwas heated under reflux for 2.5 h. After cooling, the mixture was concentrated. The residue was diluted with MeOH (100 niL) and concentrated, and this process was repeated. Ether was added to the residue and the mixture stirred for 30 minutes before filtering to give the title compound (25.9 g, 86%) as a white solid. H NNR (300 MHz, DMSO-d6) ppm 1.70-1.86 (m, 4H) 1.97-2.04 (m, 2H) 2,46-2.61 (m, lH) 2.75-2.84 (m, 2H) 8.02 (br s, 3H)

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 4426-11-3.

Reference:
Patent; Takeda Pharmaceutical Company Limited; BUFFHAM, William; CANNING, Hannah; DAVENPORT, Richard; FARNABY, William; MACK, Stephen; PARMAR, Alka; WRIGHT, Susanne; US2015/57298; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 630-18-2, name is Pivalonitrile, belongs to nitriles-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 630-18-2, Product Details of 630-18-2

General procedure: To an ice cold solution of pivalonitrile (1f, 120 muL, 1.085 mmol) in Et2O (1.0 mL)was added an ethereal solution of 2-naphthylmagnesium bromide (2b, 0.75 M, 1.88mL, 1.410 mmol) and the reaction mixture was stirred at 60 C in a sealed tube for 2 h.After cooling to 0 C, the reaction mixture was treated with anhydrous MeOH (132muL), followed by the addition of CuBr2 (24.3 mg, 0.109 mmol) and anhydrous DMF(10.0 mL). The resulting reaction mixture was stirred at 80 C under an oxygenatmosphere for 6 h. Then the reaction was quenched by the addition of pH 9ammonium buffer solution and the organic materials were extracted with Et2O. Thecombined organic extracts were washed with water, and then with brine and driedover anhydrous MgSO4. The solvents were removed in vacuo and the resulting crudematerial was purified by flash column chromatography using hexane-EtOAc (90:10)to afford 2-naphthonitrile

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, Pivalonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Tnay, Ya Lin; Ang, Gim Yean; Chiba, Shunsuke; Beilstein Journal of Organic Chemistry; vol. 11; (2015); p. 1933 – 1943;,
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