Category: nitriles-buliding-blocks

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 5866-98-8 as follows. name: 2,6-Dichloro-3-nitrobenzonitrile

To a 1 L two-neck round bottom flask was added 2,6-dichloro-3-nitrobenzonitrile (11. I g, 51.1 mmol) followed by ethyl acetate (102 mL). The flask was equipped with an internal thermometer and magnetic stir bar and cooled to 5 0C by immersion into an ice bath. Methylamine was added dropwise to the cooled reaction mixture as a 40% aqueous solution (8.9 mL, 115 mmol) with vigorous stirring. The reaction mixture was stirred for an additional 3 hours with cooling, after which more methylamine (1.8 ?iL, 23 r?mol) was added. The reaction vessel was removed from the ice bath and stirred for an additional 1.5 hours. To the reaction mixture was added water (30 mL) followed immediately by hexane (45 mL) and the resulting slurry was stirred for 15 minutes. The solid was recovered by filtration and washed with water followed by methanol to provide 6-chloro-2-methylamino-3-nitro- benzonitrile (10.49 g, 96%) as a bright yellow solid, which was used directly without further purification. 1H NMR (400 MHz, OMSO-de) delta 8.55 – 8.53 (m, IH), 8.28 (d, IH, J= 9.0 Hz), 6.95 (d, IH), J = 9.0 Hz), 3.30 (d, IH, 7= 5.5 Hz).

According to the analysis of related databases, 5866-98-8, the application of this compound in the production field has become more and more popular.

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. 68385-95-5, name is 2-Amino-3,5-dibromobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Amino-3,5-dibromobenzonitrile

General procedure: 4.3.1. General procedure for tacrine analogs. To a mixture of 2-amino-3,5-dibromobenzonitrile (1.0 mmol) and ketone (1.10 mmol) in toluene (12 mL) placed in a round bottom flask connected to a reflux condenser was added Lewis acid (1.20 mmol). The mixture was heated at 120 C for 24 h under stirring. After cooling to room temperature, the remaining solids were treated with NaOH solution (2 mol L-1, 12 mL) and this mixture was heated at reflux for 24 h. On cooling to room temperature, the reaction mixture was extracted with CHCl3 (3*25 mL), and the organic layers were combined and dried over Na2SO4. The solvent was evaporated under reduced pressure to give the desired product. The procedures were performed under an argon atmosphere in the presence of ZnCl2, InCl3, FeCl3, and BiCl3. The isolated products appeared to be sufficiently clean and no further purification was conducted.

According to the analysis of related databases, 68385-95-5, the application of this compound in the production field has become more and more popular.

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. 57381-49-4, name is 2-Bromo-4-chlorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Bromo-4-chlorobenzonitrile

Example 6A2-Bromo-4-chlorobenzylamine; 13.9 ml (13.9 mmol) of borane-THF complex (1 M) are provided with ice cooling. Slowly a solution of 604 mg (2.8 mmol) of 2-bromo-4-chlorobenzonitrile (Example 1A) in 60 ml of THF is added. Thereafter the reaction mixture is heated under reflux for 1 h, cooled, and 20 ml of 1N hydrochloric acid are added dropwise with ice cooling. For the work up, the solution is rendered alkaline with a 1N sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated on a rotary evaporator. The crude product (450 mg, about 73% pure) is reacted further without purification.1H NMR (300 MHz, CDCl3): delta=3.89 (s, 2H), 7.35-7.45 (m [ABM], 2H), 7.55 (d, 1H).

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 57381-49-4.

Application of 329314-68-3,Some common heterocyclic compound, 329314-68-3, name is 2,4-Difluoro-5-methylbenzonitrile, molecular formula is C8H5F2N, 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.

Step C – Synthesis of Compound 29C; A solution of compound 29B (1.400 g, 9.154 mmol) and hydrazine (0.700 mL, 22.3 mmol) in isopropyl alcohol (50 mL, 653.1 mmol), was heated to reflux and allowed to stir at this temperature for 24 hours. The reaction mixture was cooled to room temperature, concentrated in vacuo and the residue obtained was purified using flash column chromatography (SiO2, Acetone/Hexanes 0-> 50%) to provide compound 29C (330 mg, 22%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4-Difluoro-5-methylbenzonitrile, its application will become more common.

Electric Literature of 1953-99-7, 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. 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Tetrachlorophthalonitrile (26.6 parts by weight),m-mercaptobenzoic acid (15.4 parts by weight),To a solution of dimethylformamide (200 parts by weight),Add potassium carbonate (15 parts by weight)The reaction was allowed to proceed for 1 hour at room temperature.Subsequently, thionyl chloride (50 parts by weight) was added and reacted at 70 C. for 1 hour. After cooling to room temperature, 1-methoxy-2-propanol (10 parts by weight) was added, and the mixture was further heated to reflux for 4 hours. .After completion of the reaction, liquid separation with ethyl acetate and 1N aqueous hydrochloric acid was performed.The organic layer was concentrated and purified by silica gel column chromatography. Subsequently, sodium tungstate for the purified sample(5 parts by weight), hydrogen peroxide (30%, 6.8 parts by weight) acetic acid(5 parts by weight) and ethanol (50 parts by weight) were added and stirred at 50 C. for 5 hours. After completion of the reaction, separation and purification by silica gel column chromatography gave Intermediate A-103 (10 parts by weight).

The synthetic route of 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile has been constantly updated, and we look forward to future research findings.

76469-88-0, name is Methyl 4-(cyanomethyl)benzoate, 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 Methyl 4-(cyanomethyl)benzoate

Step 2: 2-(4-(Methoxycarbonyl)phenyl)acetic Acid A stirred solution of methyl 4-(cyanomethyl)benzoate (22.0 g, 0.125 mol) in methanol (550 mL) was bubbled through with hydrogen chloride gas for 8 h under reflux conditions. The reaction mixture was cooled to 20 C., stirred for an additional 24 h and filtered. The filtrate was evaporated under reduced pressure. The resultant residue was dissolved in diethyl ether, washed sequentially with water and saturated aqueous sodium hydrogen carbonate, dried over sodium sulfate and evaporated to afford the methyl ester as a solid residue. 1H NMR (400 MHz, CDCl3): 8.00 (d, J=8 Hz, 2H); 7.35 (d, J=8.4 Hz, 2H); 3.91 (s 3H); 3.70 (s, 3H); 3.68 (s, 2H). GCMS: 209 (M+H). The methyl ester (8.21 g, 0.039 mmol) was dissolved in methanol, treated with sodium hydroxide (1.58 g, 0.039 mol), heated to 50 C., stirred for 4 h, cooled to room temperature, stirred for an additional 24 h and concentrated in vacuo. The resultant residue was partitioned between diethyl ether and water. The aqueous layer was acidified with concentrated HCl. The resultant precipitate was removed by filtration and dried overnight, under vacuum, to afford 2-(4-(methoxycarbonyl)phenyl)-acetic acid (80%) as an off-white solid. 1H NMR (400 MHz, DSMO-d6): 7.90 (d, J=8 Hz, 2H); 7.422 (d, J=8 Hz, 2H); 3.85 (s 3H) 3.68 (s, 2H). [M+H] 195

The synthetic route of 76469-88-0 has been constantly updated, and we look forward to future research findings.

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 19924-43-7 as follows. Recommanded Product: 19924-43-7

Example 143; tert-butyl 1-isopropyl-6-((3-methoxy-6-methylpyridin-2-yl)methoxy)4-methyl-3,4-dihydroisoquinoline-2(1H)-carboxylate To a solution of methoxyphenyl acetonitrile (4.0 g, 27 mmol) in THF at room temperature was added NaH (1.19 g, 30 mmol). After 20 min, MeI (1.68 mL, 27 mmol) was added. The reaction was stirred at room temperature overnight. H2O was added to quench the reaction. It was concentrated and diluted with Ether. The ether was washed with 1N HCl, saturated NaCl, dried and concentrated to give a crude mixture which was purified by column chromatography on ISCO (120 g) with 0-30% hexanes in ethyl acetate over 28 min to yield 2-(3-methoxyphenyl)-propanenitrile (1.9 g, 44% yield) as a light brownish oil. HPLC retention time (Method C)=2.47 min. LC/MS (ESI) (M+H)+=162.16. 1H NMR (CDCl3, 400 MHz) delta ppm 1.64 (d, J=7.34 Hz, 3H), 3.82 (s, 3H), 3.85-3.92 (m, 1H), 6.83-6.96 (m, 2H), 7.24-7.34 (m, 2H).

According to the analysis of related databases, 19924-43-7, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, molecular formula is C20H23FN2O2, 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. name: 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

To a 100 mL three-necked flask equipped with a stirring blade and a thermometer were added racemic 4- [4- (dimethylamino) -1- (4′-fluorophenyl) -1-hydroxybutyl] -3- (hydroxymethyl ) -benzonitrile free form (3) 10 g (29.3 mmol),45 mL of 1-butanol (4.5 parts by volume based on 1 part by mass of the free form (3)),4.4 mL of chloroform (0.44 parts by volume based on 1 part by weight of the free form (3)) was added.The resulting mixture was heated to 60 C.,30 mL of 1-butanol (3.0 parts by volume based on 1 part by mass of the free form (3)),Acetic acid in 0.4 mL of a mixed solutionA solution of 4.5 g (11.7 mmol) of (+) – di- (p-toluoyl) tartaric acid was mixed,The free form (3) was tartarylated.After tartarylation,1-butanol 75 mL (tartrate (4)9.4 parts by volume based on 1 part by mass),While maintaining the solvent composition of 4.4 mL of chloroform (0.44 parts by volume based on 1 part by weight of tartrate (4)),Seed crystal 25 mg was added,The mixture was stirred at 60 C. for 1 hour,The precipitation of crystals was visually confirmed.After precipitation of crystals was confirmed,Cooling to 20 C at a cooling rate of 20 C / hr,Further aging was carried out at the same temperature for 3 hours to precipitate crystals.After aging, crystals precipitated by vacuum filtration were filtered off,By 1 mL of 1-butanol (1 part by volume based on 1 part by mass of the free form (3)),The filtered crystals were washed twice.The obtained white crystals were dried under reduced pressure at 40 C. for 12 hours,As white crystals(10.4 mmol) of tartaric acid salt (4) (yield: 38%Chemical purity 99.83%Impurity 1 0.002%,Impurity 2 0.015%,Optical purity 98.83%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 103146-25-4, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 135748-35-5, name is 4-Chloro-2,5-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 135748-35-5, HPLC of Formula: C7H2ClF2N

b 2-[[(1R)-3-Azido-1-(3-isoxazolyl)propyl]oxy]-4-chloro-5-fluorobenzonitrile The product from step (a) (0.1 g) and 2,5-difluoro-4-chloro-benzonitrile (0.18 g) and sodium hydride (60% dispersion in oil, 0.035 g) were subjected to the procedure described in Example 90(a) to afford the product as a gum (0.15 g). MS APCI+ve m/z 294 [(M-28)+].

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Reference of 326-62-5, These common heterocyclic compound, 326-62-5, name is 2-(2-Fluorophenyl)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.

General procedure: A mixture of nitrile (5 mmol), tert-butyl benzoate (5.5 mmol) and Zn(ClO4)2·6H2O (2 mol%) was placed in around bottom flask. Then, the reaction mixture was heated at 50 C for the given time. After completion of the reaction monitored by thin layer chromatography (TLC), the reaction mixture was quenched with 5-ml water. Then the reaction system was added 10 ml aqueous NaOH solution (1 mol/L) and continued to be stirred 5 min and extracted with ethyl acetate (3 × 10 ml). The organic layers were collected, combined, washed with water (3 × 10 ml), driedover anhydrous Na2SO4, and concentrated under vacuum.

The synthetic route of 326-62-5 has been constantly updated, and we look forward to future research findings.