Category: 3215-64-3

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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, A new synthetic method of this compound is introduced below., Product Details of 3215-64-3

A mixture of 6-chloro-4-(ethyl amino) nicotinaldehyde (Scheme 1 compound 6) (1.20 g, 6.52 mmol), 2-(2,6-dichlorophenyl)acetonitrile (1.57 g, 8.47 mmol) and K2C03 (2.70 g, 19.56 mmol) in dry DMF (12 mL) was heated to 100 C under nitrogen atmosphere for 16 h. After TLC showed the starting material was completely consumed, the reaction mixture was cooled to RT, diluted with EtOAc (100 mL), washed with water (2 x 30 mL) and brine (20 mL) then dried over Na2S04 and concentrated to give a residue which was purified by flash chromatography on silica gel (eluting with petroleum ether/EtOAc 100/0 gradually increasing to 70/30) to give 7-chloro-3-(2,6-dichlorophenyl)-l-ethyl-l,6-naphthyridin-2(lH)-imine (1.5 g, 45%) as a black gummy solid. 1H NMR (400 MHz, DMSO-d6): delta 8.45 (d, J= 4.7 Hz, 1H), 7.66 (d, J= 8.1 Hz, 2H), 7.56 (t, J= 7.2 Hz, 1H), 7.50 (s, 1H), 7.45 (s, 1H), 6.85 (d, J= 10.0 Hz, 1H), 4.30 (s, 2H), 1.22-1.16 (m, 3H). MS [ESI, MH+] = 352.05.

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; MANNKIND CORPORATION; TOLERO PHARMACEUTICALS, INC.; ZENG, Qingping; FARIS, Mary; MOLLARD, Alexis; WARNER, Steven L.; FLYNN, Gary A.; WO2014/52365; (2014); A1;,
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3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, 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. Application In Synthesis of 2-(2,6-Dichlorophenyl)acetonitrile

To a solution of 2, 6-dichloro-phenyl-acetonitrile (15. 0g, 80.62 mmol) in the dichloromethane (50 mL) and H2S04 (40 mL) is added (slowly) a mixture of H2SO4 (14 mL) and HN03 (5.5 mL) at 0C. The reaction mixture is stirred at 0C for 20 minutes, warmed to room temperature for half hour, and then concentrated to remove organic solvent. The solution is poured into a beaker containing ice-water (400 mL) to give a crystalline precipitate, which is collected by vacuum filtration and washed with water to afford the product (20.44 g, 82.4%).

The synthetic route of 3215-64-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; WO2005/34869; (2005); A2;,
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Application of 3215-64-3, 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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, This compound has unique chemical properties. The synthetic route is as follows.

5.47 g of 60% NaH are added, in 5 minutes, to 21 g of the aldehyde obtained in the previous stage, dissolved in 240 ml of DMF and cooled to 5 C., followed by 29.05 g of 2,6-dichlorophenylacetonitrile, in 20 minutes, in small fractions. The stirring is continued for 30 minutes at 5 C. and then at ambient temperature overnight. The reaction medium is cooled to 5 C. and 65 ml of a saturated NH4Cl solution and then 500 ml of a water/ice mixture are added; a red precipitate forms, which is filtered off, washed twice with water, filter-dried to a maximum, and washed with ether, with 100 ml of chloroform and then with ether again; after drying, a beige solid is obtained, Mp=250-253 C., m=29.92 g.

The chemical industry reduces the impact on the environment during synthesis 2-(2,6-Dichlorophenyl)acetonitrile. I believe this compound will play a more active role in future production and life.

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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Nitriles – Chemistry LibreTexts

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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-(2,6-Dichlorophenyl)acetonitrile

4-Methylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (22.00 g, 120.1 mmol) and 2, 6-DICHLOROPHENYLACETONITRILE (26.90 g, 144.6 mmol) were added to a dry 1 L three- necked flask equipped with an overhead stirrer. The solids were dissolved in 125 mL of dry DMF. The pale yellow solution turned slightly orange upon addition of 70 g (506 mmol) OF K2C03. The reaction was heated to 100C and stirred for 18 hours at this temperature. The reaction became dark reddish-orange in color. The flask was cooled to 50C and the resulting precipitate was filtered. The pink solid was washed with 100 mL of 3: 1 DMF/water. After vacuum drying, 13.45 g (32 %) OF 6- (2, 6-dichloro-phenyl) -8- METHYL-2-METHYLSULFANYL-8H-PYRIDO [2, 3-d] pyrimidin-7-ylideneamine were obtained. The spectral data matched literature values.

The synthetic route of 3215-64-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH; WO2004/63195; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Synthetic Route of 3215-64-3, 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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of 15.3 g (100 mmol) of 2-(2,6difluorophenyl)acetonitrile, 152.5 g (70 mL, 812 mmol) of dibromoethane, and 32.7 g (144 mmol) of Et3BnN+Cl- was isolated from moisture and carbon dioxide and vigorously stirred at 60. A solution prepared from 95 g (1430 mmol, ?84.5%) of KOH and 95 mL of water was then added dropwise; the mixture was stirred during 6 h at 60-65C, and left overnight. On the next day, the reaction mixture was extracted with t-BuOMe (3×100 mL), the combined organic fractions were evaporated, and residual water was removed via azeotropic distillation with toluene. Then 60 mL of water and 40 mL of concentrated sulfuric acid were added to the obtained 1-(2,6-difluorophenyl)cyclopropanecarbonitrile, and the mixture was refluxed during 4 h. The reaction mass was cooled to ambient; the precipitate was filtered off and dried. Yield 17.82 g (90%), mp 156-157 (toluene).

The synthetic route of 2-(2,6-Dichlorophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, A new synthetic method of this compound is introduced below., Safety of 2-(2,6-Dichlorophenyl)acetonitrile

Example 9a Preparation of 2-(2,6-dichlorophenyl)-2-methylpropanenitrile To a 1 M solution of potassium tert-butoxide (403 mL, 403 mmol) at -66 C. (acetone/dry ice) was slowly added 2-(2,6-dichlorophenyl)acetonitrile (25.0 g, 134 mmol) in anhydrous THF (150 mL). The mixture was stirred at -66 C. for 20 minutes. Then, iodomethane (33.6 mL, 538 mmol) was added drop-wise over 25 minutes at -66 C. At this stage, it was exothermic and a large amount of light yellow precipitate was observed. The suspension was stirred at -60 C. for 30 minutes. The reaction mixture was quenched with 200 mL ice water, and extracted with ether (3*150 mL). The organics were combined, washed with 150 mL brine, dried over Na2SO4, and concentrated on a rotary evaporator. The crude product (30 g, yellow oil) was purified by column chromatography (ISCO, 330 g silica, 20% EtOAc in hexanes) to afford 2-(2,6-dichlorophenyl)-2-methylpropanenitrile (28.2 g, 132 mmol, 98% yield) as a light yellowish oil. 1H-NMR (CDCl3, 400 MHz) delta 7.35 (d, 2H, J=8.03 Hz), 7.16 (t, 1H, J=8.0 Hz), 2.09 (s, 6H); 13C-NMR (CDCl3, 126 MHz) delta 134.6, 133.8, 131.4, 129.0, 124.1, 38.6, 29.2; MS m/e 214.10 (M+H+); HPLC (XBridge 5mu C18 4.6*50 mm, 4 mL/min, Solvent A: 10% MeOH/water with 0.2% H3PO4, Solvent B: 90% MeOH/water with 0.2% H3PO4, gradient with 0-100% B over 4 minutes): 3.16 minutes.

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; BRISTOL-MYERS SQUIBB COMPANY; EXELIXIS PATENT COMPANY LLC; Busch, Brett B.; Stevens, JR., William C.; Kick, Ellen K.; Zhang, Haiying; Bollu, Venkataiah; Martin, Richard; Mohan, Raju; US2015/299136; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile, A new synthetic method of this compound is introduced below., Product Details of 3215-64-3

EXAMPLE 10 2,7-Diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine (Prepared by the method of U.S. Pat. No. 3,534,039). To a solution of sodium 2-ethoxyethoxide prepared from 0.14 g of sodium and 60 mL of 2-ethoxyethanol was added 2.07 g of 2,4-diamino-5-pyrimidinecarboxaldehyde, and 2.79 g of 2,6-dichlorophenylacetonitrile. The mixture was heated at reflux for 4 hours, allowed to cool to room temperature, and the precipitated product was filtered and washed with diethyl ether to give 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]-pyrimidine, mp 325-332 C.

The synthetic route of 3215-64-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Warner-Lambert Company; US5620981; (1997); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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, Quality Control of 2-(2,6-Dichlorophenyl)acetonitrile

Example 21Example for Compound 21Into a 1 L flask was weighed 25.0 g (134 mmol) of 2,6-dichlorophenylacetonitrile and 250 mL of anhydrous THF. The resulting solution was cooled to -70 C. and 134 mL of 1.0 M potassium tert-butoxide (1.0 M) in THF was added followed by 8.4 mL of iodomethane (1.0 eq). The reaction was stirred at -70 C. for 1 h then was allowed to warm to room temperature over 3 h. The reaction was concentrated in vacuo to remove THF then was washed into a separatory funnel with ethyl acetate and 1 M HCl. The ethyl acetate was separated, washed with bisulfite, brine, was dried (Na2SO4), and concentrated in vacuo. The residue was purified by silica gel flash chromatography (Biotage, 300 g SiO2, gradient elution from 100% hexanes to 10% ethyl acetate over 1 h). Appropriate fractions were combined and concentrated in vacuo to afford the desired product as a colorless oil, 99% pure by GC, yield: 12.2 g (45%). 1H NMR (CDCl3, 400 MHz) delta 7.36 (d, J=8 Hz, 2H), 7.22 (t, J=8 Hz, 1H), 4.84 (q, J=7 Hz, 1H), 1.07 (d, J=7 Hz, 3H).

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; BRISTOL-MYERS SQUIBB COMPANY; EXELIXIS PATENT COMPANY LLC; Busch, Brett B.; Stevens, JR., William C.; Kick, Ellen K.; Zhang, Haiying; Bollu, Venkataiah; Martin, Richard; Mohan, Raju; US2015/299136; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts