Month: March 2021

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. 60758-86-3, name is 3-Ethoxy-4-methoxybenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C10H11NO2

PREPARATION 131(6) To a suspension of lithium aluminum hydride (1.17 g) in anhydrous tetrahydrofuran (15 mL) was added a solution of 3-ethoxy-4-methoxybenzonitrile (2.73 g) in tetrahydrofuran (15 mL). The mixture was stirred for an hour under water cooling and then for an hour at ambient temperature. Potassium sodium (+)-tartrate aqueous solution was added to the mixture under ice-water cooling. The mixture was diluted with ethyl acetate and the insolubles were filtered off. After evaporation of the filtrate, ethyl acetate was added. The solution was dried over magnesium sulfate and evaporated in vacuo to give 3-ethoxy-4-methoxybenzylamine as yellow oil (2.81 g). NMR (CDCl3, delta): 1.47 (3H, t, J=7 Hz), 3.80 (2H, s), 3.87 (3H, s), 4.12 (2H, q, J=7 Hz), 6.80-6.90 (3H, m).

The synthetic route of 60758-86-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6384080; (2002); B1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 455-18-5, name is 4-(Trifluoromethyl)benzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 455-18-5

100 ml of tert-amyl alcohol was placed in a 250 ml three-necked flask, and 4 g of sodium was cut into sodium pellets, and then acatalytic amount of 20-40 mg of ferric chloride was added as a catalyst. Heat to 100 ~ 105 C, the reaction 2 ~ 3h. Thetemperature was lowered to 50 to 60 C, and 68.6 mmol of the compound 2-5 was added, followed by heating to 100 to 105 C.8 ml of a mixture of diisopropyl succinate compound 1 and 40 ml of tert-amyl alcohol was added to a three-necked flask througha constant pressure dropping funnel, and the mixture was 3-5 hours after 2-3 hours. Finally, react for another 4 hours, stop thereaction, pour the reaction product into a beaker, dilute with 100 ml of methanol, add acetic acid to adjust the pH to 7, filter withsuction, wash the filter cake with methanol, take the filter cake, heat and dry, then use N, The N-dimethylformamide is thermallydissolved, cooled and suction filtered, and the filter cake is washed with water and methanol, and the filter cake is taken anddried by heating to obtain the product 3-5.

According to the analysis of related databases, 455-18-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; East China University of Science and Technology; Lily Group Co., Ltd.; Wang Limin; Li Jun; Xu Jie; Wang Feng; Wang Guifeng; Wei Xiaochuan; Wang Kang; He Yulong; Lv Jinge; Yang Qingying; Zhang Yingning; Xu Meng; Tian He; Chen Lirong; (33 pag.)CN109897043; (2019); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Some common heterocyclic compound, 83101-12-6, name is 4-(3-Hydroxypropyl)benzonitrile, molecular formula is C10H11NO, 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. SDS of cas: 83101-12-6

33C 3-(4-Cyanophenyl)propyl methanesulfonate Triethylamine (0.54 ml, 4.03 mmol) and methanesulfonyl chloride (0.30 ml, 4.03 mmol) were added to a solution of 3-(4-cyanophenyl)propan-1-ol (0.50 g, 3.10 mmol) in dry methylene chloride (15 ml), cooled at 0C and under inert atmosphere. The reaction mixture was stirred at 0C for 2 hours, after that was diluted with methylene chloride (50 ml), washed in succession with 0.05M HCl, with a NaCl saturated solution, dried and the solvent was evaporated off. 0.675 g of the title compound were obtained as a semi-solid oil (94% yield). 1H N.M.R. (300 MHz, CDCl3) delta ppm: 1.89 (m, 2H); 2.63 (t, 2H); 2.85 (s, 3H); 4.05 (t, 2H); 7.14 (d, 2H); 7.38 (d, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 83101-12-6, its application will become more common.

Reference:
Patent; LABORATORIOS MENARINI S.A.; EP775133; (2001); B1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Synthetic Route of 425379-16-4, 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 425379-16-4 as follows.

2-Bromo-3-fluorobenzonitrile (1 .0 g, 5.0 mmol) and (1 H-pyrazol-5-yl)boronic acid (647 mg, 4.6 mmol) were combined and dissolved in degassed DME (15 ml_) then treated with NaHCO3 (1260 mg, 8.4 mmol) in water and the reaction purged with bubbling N2 for 5 minutes. The reaction was treated with Pd(PPh3) (288 mg, 0.2 mmol) and then purged with bubbling for 5 minutes in a sealed vessel and then heated to reflux for 2 h. Cooled to 23 C filtered and solid rinsed with EtOAc and the layers separated. The organic layers were combined, dried and concentrated under reduced pressure.Chromatography (0-30% ethyl acatate / hexanes) afforded 3-fluoro-2-(1 H- pyrazol-5-yl)benzonitrile (178 mg,19%).

According to the analysis of related databases, 425379-16-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; WO2011/50200; (2011); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

These common heterocyclic compound, 6306-60-1, name is 2-(2,4-Dichlorophenyl)acetonitrile, 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. Safety of 2-(2,4-Dichlorophenyl)acetonitrile

A suspension of sodium hydride (2.16 g) in dry dimethylsulphoxide (DMSO: 70 ml) was stirred at 50 C. under a nitrogen atmosphere for 2.5 hours and then cooled to 15 C. in an ice bath. A mixture of 2,4-dichlorophenylacetonitrile (8.37 g) and 3-methanesulphonyloxyhex-1-yl methanesulphonate (14.27 g) in DMSO (70 ml) was added dropwise to this solution over 15 minutes. The reaction mixture was stirred at room temperature for 0.5 hours, at 90 C. for 3 hours, and at 130 C. for 2 hours, and was then allowed to cool, diluted with water, and extracted with ether. The extracts were washed with water, dried over magnesium sulphate and concentrated to give a dark coloured oil (7.76 g). Purification of this crude product by bulb-to-bulb distillation gave a mixture of diastereomers of 1-cyano-1-(2,4-dichlorophenyl)-3-prop-1-ylcyclopentane (4.95 g, 39%) as a colourless oil (oven temperature: 230 C., ca. 10 torr).

The synthetic route of 2-(2,4-Dichlorophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Imperial Chemical Industries Plc; US4684396; (1987); A;,
Nitrile – Wikipedia,
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. 1735-88-2, name is 2-Cyano-N-(4-fluorophenyl)acetamide belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C9H7FN2O

EXAMPLE 7; Preparation of3-(5-trifluoromethyl-l, 2, 4-oxadiazol-3-yl)-l-(4-fluorophenyl)-5- methylene-2-oxo-4-methyl-2,5-dihydro-lH-pyrrole (Compound 245); The following compounds were prepared according to reaction schemes 7 and 12.(a) A mixture of iV-(4-fluorophenyl)cyanoacetamide (1 equiv.), hydroxylamine hydrochloride (2 equiv.) and triethylamine (2 equiv.) in DMF was heated to 50-600C for 4 h then diluted with water and the product filtered off and dried.

The synthetic route of 1735-88-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COMMONWEALTH SCIENTIFIC AND INDUSTRIAL RESEARCH ORGANISATION; WO2008/70934; (2008); 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. 2032-34-0, name is 3,3-Diethoxypropanenitrile, A new synthetic method of this compound is introduced below., Formula: C7H13NO2

7-(benzyloxy)quinoline-3-carbonitrile (113): 113 was prepared according to the procedure of Cai T.B., et ad journal of Medicinal Chemistry, 51:1849-1860, 2008. Characterization data for 113: < (500MHz, CDC13) 5.28 (s, 2H), 7.39-7.51 (m, 5H), 7.65 (dd, 1H, J 2.5 Hz and 9.0 Hz), 8.05 (d, 1H, J 9.0 Hz), 8.14 (d, 1H, / 2.5 Hz), 8.63 (d, 1H, J 2.0 Hz), 9.15 (d, 1H, J 2.0 Hz) <5C (500MHz, CDC13) 70.6, 116.3, 121.7, 122.3, 122.8, 123.1, 123.3125.4, 127.7, 128.5, 129.5, 130.8, 141.2, 149.1, 151.4. The synthetic route of 2032-34-0 has been constantly updated, and we look forward to future research findings. Reference:
Patent; HARO PHARMACEUTICAL INC.; THE ROYAL INSTITUTION FOR THE ADVANCEMENT OF LEARNING/MCGILL UNIVERSITY; UNIVERSITE DE MONTREAL; BETTOUN, David; MARTINEZ, Eduardo, J.; GLEASON, James; MADER, Sylvie; XING, Shuo; (72 pag.)WO2015/188015; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

1835-65-0, name is 3,4,5,6-Tetrafluorophthalonitrile, 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. HPLC of Formula: C8F4N2

First raw material 4,5-bis (pentafluorophenyl) -3,6-difluoro-phthalonitrile were prepared as follows: A 200ml reaction vessel equipped with a dropping funnel and a thermometer tetrafluorophthalonitrile 20.1 g ( 100.45mmol), potassium fluoride 13.99g (240.79mmol), was added to the methyl isobutyl ketone 130ml.After cooling with an ice-bath, conducted from the dropping funnel, was added slowly a solution of pentafluorophenol 37.0g (201.02mmol) of methyl isobutyl ketone 70 ml, then the reaction was stirred for 2 days at room temperature It was.Except inorganic salt and the reaction solution was filtered, washed with water using a separatory funnel, was dehydrated with anhydrous sodium sulfate, the reaction solution was concentrated in an evaporator.The concentrate, by re-precipitation purification with toluene / hexane solvent, 4,5-bis (pentafluorophenyl) -3,6-difluoro phthalonitrile, 70.83percent yield (37.4g, 70.81mmol obtained in).

The synthetic route of 1835-65-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ehime University; Nippon Shokubai Co.,Ltd.; Uno, Hidemitsu; Masuda, Tsuyoshi; (27 pag.)JP5656235; (2015); B2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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 120315-65-3 as follows. Recommanded Product: 120315-65-3

Preparation 42 tert-butyl 2-(4-cyano-2 methoxyphenyl)acetate [0219] Combined (2-(tert-butoxy)-2-oxoethyl)zinc(II) chloride (4.24 mL, 2.122 mmol) and 4-bromo-3-methoxybenzonitrile (0.30g, 1.42 mmol) in THF (4.29 mL), then 2′- (dicyclohexylphosphino)-N,N-dimethyl-[l, l’-biphenyl]-2-amine (0.056 g, 0.141 mmol) and Pd(dba)2 (0.041 g, 0.071 mmol) were added and the reaction was refluxed at 100C overnight. The reaction mixture was concentrated down by rotary evaporation and purified on a silica gel column eluting with hexanes and EtOAc to give the title compound as a yellow oil (102 mg, 29%). MS m/z [M+H]+ 248.

According to the analysis of related databases, 120315-65-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; BROWN, Jason, W.; DAVIS, Melinda; IVETAC, Anthony; JONES, Benjamin; KIRYANOV, Andre, A.; KUEHLER, Jon; LANIER, Marion; MIURA, Joanne; MURPHY, Sean; WANG, Xiaolun; WO2014/160810; (2014); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Electric Literature of 67237-76-7, 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. 67237-76-7, name is Ethyl 2-(2-cyanophenyl)acetate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 250 ml four-necked flask with stirring, thermometer and distillation system,23.3 g (0.1 mol) of N-phenyl-2-chloro-2-(pyridin-2-yl)ethylamine (II2) (commercially available) was added.20.5 g (0.11 mol) of ethyl 2-cyanophenylacetate, reacted at 105-110 C for 4 hours.At the same time, the removed ethanol is distilled off, and the gas phase detection reaction is completed. Cool down to 50-60 C,Add 50 g of methyl tert-butyl ether, cool to room temperature, and filter.The filter cake was washed with 20 g of methyl tert-butyl ether and dried.33.8 g of N-phenyl-N-[2-chloro-2-(pyridin-2-yl)]ethyl-2-cyanophenylacetamide (IV2) were obtained.The yield was 89.8%, and the gas phase purity was 99.6%.

The synthetic route of Ethyl 2-(2-cyanophenyl)acetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Ju Lizhu; Zhang Mingfeng; (10 pag.)CN110028442; (2019); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts