Month: April 2021

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.

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.

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.

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.

Application of 621-03-4,Some common heterocyclic compound, 621-03-4, name is 2-Cyano-N-phenylacetamide, molecular formula is C9H8N2O, 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: To a solution of NaOEt (3.0 mmol) in anhydrous ethanol (10 mL) were added amide (2.0 mmol) and 2-aryl vinamidinium salt (2.0 mmol) at room temperature. The reaction mixture was stirred at the same temperature for 24 h. After completion of the reaction, the reaction mixture was poured into water (100 mL) to precipitatethe crude product, which was collected by filtration and washed with water. The residue was purified by silica gel column chromatography(CH2Cl2:MeOH) to afford the corresponding 1,5-diarylpyridin-2(1H)-one.

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

Electric Literature of 29509-06-6,Some common heterocyclic compound, 29509-06-6, name is 4-Methyl-3-oxopentanenitrile, molecular formula is C6H9NO, 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 B22 To a stirring suspension of 6-aminobenzothiazole (0.500 g, 3.33 mmol) in cone. HCl (5 ml) at 0-5 C. was added a solution of NaNO2 (0.276 g, 3.99 mmol) in H2O (5 ml). The mixture was stirred at 0-5 C. for 75 min until a clear yellow solution was obtained. To this was then added a solution of SnCl2.2H2O (2.76 g, 13.3 mmol) in conc. HCl (5 ml). After completing the addition, the suspension was stirred at RT for 2 h. 4-Methyl-3-oxopentanenitrile (0.444 g, 3.99 mmol) and EtOH (50 ml) were added and the reaction was stirred with heating at 75 C. After 18 h, the completed reaction was cooled to RT and concentrated to an aqueous residue. This was chilled thoroughly in ice and made strongly basic (pH 12-13) by the addition of 6M NaOH. While still cold the mixture was extracted with EtOAc (2*). The combined organics were washed with H2O (2*), brine (1*), dried (MgSO4), filtered and evaporated to afford crude 1-(benzo[d]thiazol-6-yl)-3-isopropyl-1H-pyrazol-5-amine (0.8 g, 93% yield) as an oil which was used as is in the next reaction. 1H NMR (400 MHz, DMSO-d6) delta 9.36 (s, 1H), 8.30 (d, J=2.4 Hz, 1H); 8.10 (d, J=8.8 Hz, 1H), 7.74 (dd, J=2.4 and 8.8 Hz, 1H), 5.36 (s, 1H), 5.33 (brs, 2H), 2.76 (septet, J=6.8 Hz, 1H), 1.17 (d, J=6.8 Hz, 6H); MS (ESI) m/z: 259.0 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Methyl-3-oxopentanenitrile, its application will become more common.

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. 21524-39-0, name is 2,3-Difluorobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 2,3-Difluorobenzonitrile

To a solution of 7-hydroxy-2-(4-(1-methyl-1H-pyrazol-9-yl}benzyl)isoindolin-1-one (0.050 g) obtained in Reference Example 6 in DMF (2 mL) was added potassium tert-butoxide (0.018 g), and the mixture was stirred under an argon atmosphere at room temperature for 30 min. To the reaction solution was added 2,3-difluorobenzonitrile (0.024 g), and the mixture was stirred at 50C for 6 hr. The reaction mixture was diluted with ethyl acetate, and washed with saturated brine. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated. The residue was crudely purified by NH silica gel chromatography (hexane-ethyl acetate), and solidified with hexane-ethyl acetate to give the title compound (0.035 g). MS: [M+H]+ 439.2 1H NMR (400 MHz, DMSO-d6) 5 3.85 (3H, s), 4.41 (2H, s), 4.66 (2H, s), 6.84 (1H, d, J = 8.3 Hz), 7.27 (2H, d, J = 8.1 Hz), 7.33 (1H, d, J = 7.3 Hz), 7.46-7.58 (4H, m), 7.77-7.86 (3H, m), 8.12 (1H, s).

The synthetic route of 21524-39-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 50397-74-5, 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. 50397-74-5, name is 4-Amino-3-bromobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 1 :- Preperation of (E)-methyl 3-(2-amino-5-cyanophenyl)acrylate To a mixture of 4-amino-3-bromobenzonitrile (10.0 g, 0.050 mmol) and methyl acrylate (9.19 mL, 0.101 mmol) in acetonitrile (200 mL) was added palladium acetate (0.568 g, 0.0025 mmol) and tri-o-tolyl phosphine (1.54 g, 0.005 mmol) and Et3N (14.64 mL, 0.105 mmol). The reaction mixture was heated to reflux for 48 h. The reaction mass was filtered through celite and washed the bed with ethyl acetate. The filtrate was concentrated to afford 6.0 g of title product. 1H NMR (300 MHz, DMSO): delta 7.92 (s, 1H), 7.82-7.77 (d, = 15.6 Hz, 1H), 7.41-7.38 (d, = 8.7 Hz, 1H), 6.77- 6.74(d, = 8.7 Hz, 1H), 6.64 (s, 2H), 6.56-6.51 (d, = 15.6 Hz, 1H), 3.70 (s, 3H).

The synthetic route of 4-Amino-3-bromobenzonitrile has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 302912-31-8, name is Ethyl 2-(4-cyanophenyl)-2-oxoacetate, 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 302912-31-8

To a solution of ethyl (4-cyanophenyl)(oxo)acetate (5.0 g, 24.6 mmol) in water (100 mL) was added concentrated hydrochloric acid (100 mL). The solution was heated to reflux for 16 hours. The solution was cooled to ambient temperature and the solids were filtered and dried to give 4- (carboxycarbonyl)benzoic acid as a white solid. ESIMS calcd 195.0 (M+ + H), found 195.0 (M+ + H).

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

Synthetic Route of 1897-52-5, The chemical industry reduces the impact on the environment during synthesis 1897-52-5, name is 2,6-Difluorobenzonitrile, I believe this compound will play a more active role in future production and life.

Take 2 L four bottles, add 600 mL of 60% sulfuric acid, electric stirring by adding 2,6_ difluorobenzonitrile 139.0 g (1.0 mol). Under N2 protection, the control reaction temperature was below 35 C, and 250 mum g of KBr03 (1.5 mol) was added to 10 batches. TLC monitoring, reaction 5-6 days, until the raw material point disappears, stop the reaction, the preparation of 800 mL 20% ice salt solution, the reaction solution Into the ice salt. After the product settling, the rapid filtration, the orange crude products, with CC14 dissolved crude products, respectively, with 5% Of NaHS03 solution, saturated Na2C03 solution and water to the solution was neutral, dried over anhydrous sodium sulfate, the solution was filtered, the water bath 60 C steamed to obtain light yellow liquid, rest for some time to cool into a pale yellow solid, vacuum distillation, warm water condensing steam, oil The bath was heated to 90 C and the fraction at a steam temperature of 58-62 C was cooled to give a white solid product in 71% 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, 2,6-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.