Category: nitriles-buliding-blocks

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. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: nitriles-buliding-blocks

The experiment examples are carried out in a 1 l reactor (10×2000 mm), equipped with feed pumps for solvent, ammonia and nitrile ester, charged with 250 ml of steel rings in the lower and upper reactor section, and centrally with 500 ml of tablets (5×3 mm) of a hydrogenation catalyst of the following composition: 28% NiO, 28% CoO, 13% CuO and 31% ZrO2, in liquid phase mode. The reduction procedure of the catalyst is as follows: the reactor is heated to 180 C. at a hydrogen feed of 50 l/h within 5 hours, then kept at 180 C. with 50 l/h of hydrogen for 20 hours, cooled under hydrogen and purged with MeOH, before ammonia and reactant and also solvent are fed in. The steel rings in the lower part of the reactor serve as the delay time zone for the amidation. 11 equivalents of hydrogen are fed in per nitrile used. The delay time is thus approx. 10 minutes.Example 9503 g/h of MeOH and, as the nitrile ester, methyl 2-cyano-2,2-dimethylacetate (in a weight ratio of 1:1) and 670 g of ammonia (20 equivalents of ammonia based on nitrile ester) are conducted through the reactor at 200 bar and 100 C. The volume space velocity is 0.5 kg/l*h. The effluent analysis shows (calculated without solvent) 99.89% aminopivalinamide, 0.03% methyl aminopivalate and 0.08% others. The delay time is approx. 9.8 minutes.

The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 64248-62-0, name is 3,4-Difluorobenzonitrile, molecular formula is C7H3F2N, 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. Recommanded Product: 3,4-Difluorobenzonitrile

Pyrrole (2, 6, 6-trimethyltetrahydroindol-4-one) (1.0 g, 5.6 iranol) and 3, 4-difluorobenzonitrile (785 mg, 5.6 mmol) were dissolved in anhydrous DMF (20 mL) . To this NaH (95%, 270 mg, 11.2 mmol) was added and stirred at 50 0C for 30 min. The reaction mixture was cooled to RT and washed with H2O and EtOAc. The organic layer was dried over MgSO4. Column chromatography on silica eluting with EtOAc-hexanes (1:1) gave the product as a yellow solid (100% clean by LCMS, product M+H = 397.1) .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 64248-62-0, its application will become more common.

Application of 15760-35-7, A common heterocyclic compound, 15760-35-7, name is 3-Methylenecyclobutanecarbonitrile, molecular formula is C6H7N, 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.

(a) 50 g (0.54 mol) of 3-methylenecyclobutanecarbonitrile are dissolved in 600 ml of water and 50 ml of ether, cooled to 5 C., and 100 mg (0.4 mmol) of osmium(IV) oxide are added. 260 g (1.2 mol) of sodium periodate are then added in portions at the temperature indicated, and the mixture is allowed to warm to RT. The organic phase is extracted with dichloromethane and, after drying and evaporation, chromatographed over silica gel, giving 25 g (49%) of 3-oxocyclobutanecarbonitrile as colourless crystals (m.p. 51 C.).

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.

Electric Literature of 26391-06-0, 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 26391-06-0 as follows.

To a solution of N, N-diethylcyanoacetamide(14.1 g, 0.1 mol) in toluene was added 0.2 g IRA 96 resin and isonitrovanillin (19.7g, 0.1 mol). The mixture was heated to reflux with azeotropic distillation of water. The reaction was continued until a TLC test showed completion of reaction.The mass was filtered hot. The filtrate was concentrated under vacuum to give the crude product, which wasre crystallized from absolute alcohol to afford 13. 61% isolated yield as light yellow solid. MR: 175-176C;1H-NMR (400 MHz, DMSO): delta 1.13 (br s, 6H), 3.39(br s, 4H), 3.92 (s, 3H), 7.67 (s, 1H), 7.76 (d, J=2.1Hz,Ar-H), 7.78 (d, J=2.1Hz, Ar-H), 10.98 (br s,-OH); ms:m/z 318.1 (negative mode).

According to the analysis of related databases, 26391-06-0, the application of this compound in the production field has become more and more popular.

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.

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.

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.

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 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.

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.