Month: April 2021

Adding a certain compound to certain chemical reactions, such as: 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, 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 3215-64-3, SDS of cas: 3215-64-3

The compound 2 – (2, 6 – dichlorophenyl) b nitrile (3.06 g, 16.4 mmol) dissolved in DMF (60 ml) in, then added to the reaction solution in the t – BuOK (1.84 g, 16.4 mmol), heating to 50 C, stirring reaction for 50 minutes, then slowly added to the reaction solution in 5 – bromo -1 – (phenyl-sulfonyl) – 1H – pyrrolo [2, 3 – b] pyridine -3 – formaldehyde (5 g, 13.7 mmol) in DMF (100 ml) solution, 1.5 hours after the completion of the dropping, the reaction solution in 50 C stirring overnight, then cooling to room temperature, the addition of water (20 ml) quenching the reaction, concentrated under reduced pressure, then adding EtOAc (200 ml) and water (100 ml) diluted residue, for a mixture of EtOAc (100 mLx 3) extraction, the combined organic phase for salt water (200 ml) washing, anhydrous Na2 SO4 Drying, concentrated under reduced pressure, the residue by silica gel column chromatography (PE/EtOAc (v/v)=4/1) to obtain the title compound (1 a and 1 b of the mixture) as a yellow solid (1.26 g, 24%).

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-(2,6-Dichlorophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; (88 pag.)CN104119331; (2018); B;,
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Synthetic Route of 3215-64-3,Some common heterocyclic compound, 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, molecular formula is C8H5Cl2N, 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.

EXAMPLE 17 6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]-pyrimidin-7-ylideneamine Powdered potassium carbonate (0.8 g; 5.8 mmol) was added to a solution of 0.220 g (1.2 mmol) of the aldehyde from Example 18 and 0.235 g (1.26 mmol) (ca. 5% excess) of 2,6-dichlorophenylacetonitrile in 2.0 mL of dimethylformamide. The mixture was heated with stirring at 125 C. for 6 hours. Ethyl acetate (5 mL) was added to the cooled mixture, and the solids were filtered and washed with ethyl acetate. The filtrate was concentrated under reduced pressure. The residual gum was triturated with 10 mL of water, and the resulting solid was filtered, washed well with water, and dried. This crude material was chromatographed by placing a chloroform solution on a silica gel column wet with chloroform. The column was eluted with 1:1 (v/v) hexane:ethyl acetate, collecting the fractions that contain the Rf 0.25 spot on tlc (1:1 hexane:ethyl acetate). Evaporation of the solvents gave a solid. The solid product was dissolved in about 0.5 mL of methylene chloride. Crystals develop. Petroleum ether (ca. 2 mL) was added, and the crystals were filtered to provide 0.168 g (40%) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-ylideneamine, mp 198-200 C. Mass spectrum (CI) 351 (M+1). Analysis calculated for C15 H12 Cl2 N4 S: C, 51.29; H, 3.44; N, 15.95. Found: C, 51.31; H, 3.41; N, 15.73.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(2,6-Dichlorophenyl)acetonitrile, its application will become more common.

Reference:
Patent; Warner-Lambert Company; US5945422; (1999); 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. 1009-35-4, name is 4-Fluoro-3-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C7H3FN2O2

4-Fluoro-3-nitrobenzonitrile (1) (2 g, 0.012 mol) in ethyl acetate(50 mL) was supplemented with stannous chloride (11.4 g,0.06 mol). The reaction mixture was stirred for 30 min and then a saturated solution of sodium hydrogenocarbonate (100 mL) was added. This mixture was treated with ethyl acetate (300 mL) andthe aqueous layer was separated. The ethyl acetate layer was evaporated under reduced pressure. The crude product was dissolved in methanol, and ice was added; the resulting precipitate was collected by filtration (Yield: 30e60%).

The synthetic route of 1009-35-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bambi-Nyanguile, Sylvie-Mireille; Hanson, Julien; Ooms, Annie; Alpan, Lutfiye; Kolh, Philippe; Dogne, Jean-Michel; Pirotte, Bernard; European Journal of Medicinal Chemistry; vol. 65; (2013); p. 32 – 40;,
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Some common heterocyclic compound, 10406-25-4, name is 4-(Aminomethyl)benzonitrile, molecular formula is C8H8N2, 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. HPLC of Formula: C8H8N2

General procedure: To a solution of benzylamine (0.6 mmol), indole (1.0 mmol) and CuI (0.1 mmol ) in CH3CN (1 mL) was added TEMPO (0.15 mmol) under atmosphere and the mixture was stirred at room temperature for overnight. The reaction mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (eluent: EtOAc/PE = 1:4) to yield the corresponding product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10406-25-4, its application will become more common.

Reference:
Article; Liao, Meixiang; Zhang, Xiaoyun; Yue, Pengfei; Synthetic Communications; vol. 48; 13; (2018); p. 1694 – 1700;,
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1897-52-5, name is 2,6-Difluorobenzonitrile, 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. COA of Formula: C7H3F2N

4.5 g of 2,6-difluorobenzonitrile and 45.3 g of xylene were added to a 200 mL four-necked flask under nitrogen atmosphere at room temperature and stirred, then 21.7 g of a methylmagnesium chloride solution (3.0 M THF solution) was added at room temperature Was added dropwise over 1 hour. The resulting mixture was stirred at room temperature for 19 hours,Was added dropwise to 31.5 g of a 20% sulfuric acid aqueous solution.The obtained mixture was heated to 50 C. and liquid separation was carried out,9.1 g of water was added to the organic layer, and the mixture was separated at 50 C.The obtained organic layer was analyzed by a high performance liquid chromatograph internal standard method, and 4.8 g of 2,6-difluoroacetophenone was confirmed to be contained (yield 95%)

The synthetic route of 1897-52-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Corporation; Ito, Tadataka; Hiraguri, Natsuru; (7 pag.)JP2016/169165; (2016); A;,
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Reference of 34662-29-8, 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. 34662-29-8, name is 3-Chloro-4-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 3-chloro-4-nitrobenzonitrile (3 g, 16.4 mmol, Chem. Pharm. Bull., 1992, 2399-2404), 2-phenylethanamine (2.5 ml, 19.7 mmol) and potassium carbonate (3.4 g, 24.6 mmol) in ethanol (200 ml) was refluxed for 5 hr. To the mixture was added 2 N aqueous NaOH (100 ml) and the whole was extracted with ethyl acetate (100 ml¡Á2). The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (hexane/ethyl acetate=1/8 as eluent) to afford the titled compound as a yellow solid (936 mg, 21%). [0371] 1H-NMR (CDCl3) delta:8.49 (d, J=2.0 Hz, 1H), 8.43 (br.s, 1H), 7.57 (dd, J=2.2, 8.8 Hz, 1H), 7.24-7.39 (m, 5H), 6.89 (d, J=9.0 Hz, 1H), 3.58-3.65 (m, 2H), 3.04 (d, J=7.1 Hz, 2H) ppm.

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-Chloro-4-nitrobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ando, Kazuo; Kawai, Makoto; Kawamura, Mitsuhiro; Matsumizu, Miyako; Morita, Asato; Sakurada, Isao; US2004/204409; (2004); A1;,
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These common heterocyclic compound, 17417-09-3, name is 2-Fluoro-5-nitrobenzonitrile, 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. Product Details of 17417-09-3

6A: 2-(Ethylsulfonyl)-5-nitrobenzonitrile; [00219] Ethanethiol (2.8 mL, 38 mmol) was added to a solution of 2-fluoro-5- nitrobenzonitrile (5.00 g, 30.1 mmol) and triethylamine (9.3 mL, 67 mmol) in DMF (100 mL). The reaction mixture was stirred for 1 h and then poured into water (500 mL). The resulting precipitate was isolated by filtration, dissolved in DCM, washed with water and brine, dried (MgSO^, and concentrated under reduced pressure. The residue (6.14 g) was dissolved in DCM (100 mL), cooled to 0C, and treated with MCPBA (16.0 g, 71 mmol) in one portion. The reaction mixture was allowed to stir at rt overnight, and then was extracted with sodium bicarbonate solution (saturated), sodium bisulfite solution (10%), and brine. The organic layer was dried (MgSO4) and concentrated under reduced pressure to afford 6A (5.6 g, 80%) as a pale yellow solid. IH NMR (400 MHz, CDCl3) delta 1.02 (s, 6H), 1.97 (m, 2H), 2.36 (t, J = 7.5 Hz, 2H), 2.68 (t, J= 7.7 Hz, 2H), 3.76 (s, 4H), 7.18 (d, J= 7.9 Hz, 2H), 7.72 (d, J= 7.5 Hz, 2H).

The synthetic route of 2-Fluoro-5-nitrobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/76431; (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. 2469-99-0, name is 3-Oxobutanenitrile, A new synthetic method of this compound is introduced below., Product Details of 2469-99-0

General procedure: 3-Acetyl-2-aminothiophene Derivatives; General Procedure Carbonyl compound (0.025 mol) was added to freshly prepared cya-noacetone (0.03 mol) in either MeOH or EtOH (40 mL). Sublimed sul-fur S8 (0.03 mol) and piperidine (0.03 mol) were added and the mix-ture was stirred and heated to 55-65 C for 24 h. Ice was then addedand the formed precipitate was filtered under vacuum and washedwith water. The obtained solid was crystallised from a suitable sol-vent, with the exception of 4g and 4j, which were collected directlywithout further purification.

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; Abdelwahab, Ahmed B.; Hanna, Atef G.; Kirsch, Gilbert; Synthesis; vol. 48; 17; (2016); p. 2881 – 2888;,
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Adding a certain compound to certain chemical reactions, such as: 21524-39-0, name is 2,3-Difluorobenzonitrile, 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 21524-39-0, Quality Control of 2,3-Difluorobenzonitrile

General procedure: A solution of 2 (1 mmol) and 3(1 mmol) in anhydrous DMF (10 mL) containing anhydrous K2CO3 (2 mmol) was heated at a given temperature for 2-36 h. DMF was removed in vacuo and the residue was dissolved in chloroform (10 mL). This solution was extracted with 5% HCl (2 x 5 mL). The combined aqueous extracts were neutralized with 10% aqueous NaOH to pH 8 and the resulting precipitate was filtered off, washed with water and dried in vacuo at 50 C for 24 h to provide analytically pure title compounds.

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, 2,3-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Karamysheva, Kseniya; Reutskaya, Elena; Sapegin, Alexander; Dorogov, Mikhail; Krasavin, Mikhail; Tetrahedron Letters; vol. 56; 41; (2015); p. 5632 – 5636;,
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Synthetic Route of 3939-09-1, 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 3939-09-1 as follows.

2,4-Difluorobenzonitrile (2.78 g, 20 mmol) and 3,4,5-trimethoxybenzylamine (3.94 g, 20 mmol) are combined and heated at 140 C for 40 m. The mixture is allowed to cool to RT and is then dissolved in TFA (20 mL) and stirred at RT overnight. The mixture is then concentrated on the rotavap and partitioned between 1N NaOH (enough till basic, ~100 mL) and ethyl acetate (100 mL). The organic layer is removed and the aqueous layer is extracted with more ethyl acetate (100 mL). The combined layers are washed with brine (50 mL), dried (MgSO4) and concentrated to an oil. The mixture is chromatographed (10 to 40%, EtOAc in hexanes) giving the isomers as two well separated products. The later eluding product is concentrated to give 4-Amino-2-fluoro-benzonitrile (1.07 g, 39%) as a white solid. (LC/MS m/z=177.8 for M+H+acetonitrile)

According to the analysis of related databases, 3939-09-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Huang, Kenneth He; Hughes, Philip; Ma, Wei; Ommen, Andy; Woodward, Angela; Veal, James; Barta, Thomas; US2008/76813; (2008); A1;,
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