Month: April 2021

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.

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.

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.

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.

Electric Literature of 51762-67-5, 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 51762-67-5 as follows.

3-Nitrophthalonitrile (1.73 g, 0.01 mol) and 4-tert-butylphenol (1.50 g, 0.01 mol) were dissolved in DMSO (30 mL), LiOH (0.42 g,0.01 mol) was then added. The resulted mixture was then stirred at 50 C for 24 h under N2 atmosphere. The product solution was cooled and then poured into NaCl solution (10% aqueous, 100 mL), the precipitated solid was filtered, washed with water and dried under vacuum. White needles were obtained after recrystallization in toluene. Yield: 51%. m.p. 116-118 C. IR (KBr), nu(cm-1): 3083, 3014, 2232 (C?N), 1695, 1632, 1563, 1506, 1485, 1465, 1429, 1386, 1351, 1275 (C-O-C), 1258, 1222, 1165, 1142, 1015, 938, 917. 1H NMR (400 MHZ, CDCl3, ppm): delta 1.353 (s, 9H, t-butyl), 6.992 (d, 2H, J=7 Hz, Ar-H), 7.245 (d, 1H, J=6 Hz, Ar-H), 7.510 (d, 2H, J=7 Hz, Ar-H), 7.799 (m, 2H, Ar-H), 7.835 (m, 1H, Ar-H). MS, m/z: 298.95 [M+Na]+.

According to the analysis of related databases, 51762-67-5, the application of this compound in the production field has become more and more popular.

Related Products of 63069-50-1, The chemical industry reduces the impact on the environment during synthesis 63069-50-1, name is 4-Amino-3-fluorobenzonitrile, I believe this compound will play a more active role in future production and life.

4-Amino-3-chloro-5-fluorobenzonitrile A mixture of 4-amino-3-fluorobenzonitrile (1 equiv.) and N-chlorosuccinimide (1.5 equiv.) in acetonitrile (0.24 M) was stirred at 85 C. for 5 h. The solvent was removed by concentration and the residue was partitioned between ethyl acetate and 5% NaOH. The organic phase was washed with 5% NaOH and brine. Then the organic phase was dried over MgSO4 and dried in vacuum to afford 4-amino-3-chloro-5-fluorobenzonitrile (88%) as a beige solid. 1H NMR (400 MHz, CDCl3) delta ppm: 7.41 (t, J=6 Hz, 1H), 7.24 (dd, J=1.8, 10.2 Hz, 1H), 4.66 (s, 2H).

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, 4-Amino-3-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

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.

To a 100 mL flask was added the solid (4- (biphenyl-2-ylamino) -3,5,6-trichlorophthalonitrile) (1.0 g), 3,4,5,6-Tetrachlorophthalonitrile (0.67 g), 1,8-Diazabicycloundec-7-ene (1.5 g) and 1-pentanol (15 mL). Thereafter, zinc acetate (0.23 g) is added and refluxed with heating. After completion of the reaction, the solvent was removed,Purify by chromatography. Dichloromethane was appropriately added to the obtained solid to dissolve the solid, and hexane was added to obtain crystals. At this time, the obtained solid was filtered and dried under vacuum to obtain a compound represented by the following general formula (8).

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, 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, other downstream synthetic routes, hurry up and to see.

Reference of 149793-69-1,Some common heterocyclic compound, 149793-69-1, name is 3-Fluoro-5-(trifluoromethyl)benzonitrile, molecular formula is C8H3F4N, 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.

In a 500-mL, 3N round-bottomed flask equipped with anlOO-mL pressure- equalizing addition funnel fitted with a nitrogen inlet, and a rubber septum, 3-fluoro-5- (trifluoromethyl)benzonitrile (8.0 g, 1.0 eq.), in acetone (40 mL). Sodium thiomethoxide (3.42 g, 1.15 eq) was dissolved in water to make 21% aqueous solution and was added dropwise in 30 min at 5C temperature. The temperature of the reaction was slowly raised to RT and stirred for 3 h. Then temperature was raised to 50-60C and maintained for further 4-6 h. The progress of the reaction was followed by TLC analysis on silica gel with 10% MeOH – DCM as mobile phase and visualization with UV, SM Rf=0.40 and Product Rf=0.25. Reaction was stirred for 3 hr at 25C and 4-6 Hrs at 50-60C and reaction mixture was transparent. The reaction mass was quench by water and extracted by ethyl acetate (3×100 mL). The combined organic layer was washed with brine 50 mL and dried over sodium sulphate and evaporated on buchi rotaevaporator. The resulting crude compound White (8 g) was subjected to further stage Yield (80.9 %).Mass: (ES+) 235.94 (M+l).

The synthetic route of 149793-69-1 has been constantly updated, and we look forward to future research findings.

Electric Literature of 4426-11-3,Some common heterocyclic compound, 4426-11-3, name is Cyclobutanecarbonitrile, molecular formula is C5H7N, 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 116A 1-[4-(trifluoromethyl)pyridin-2-yl]cyclobutanecarbonitrile 2-Fluoro-4-(trifluoromethyl)pyridine (0.731 mL, 6 mmol) and cyclobutane-carbonitrile (0.841 mL, 9.00 mmol) were dissolved in toluene (10 mL). 0.5M KHMDS (18.00 mL, 9.00 mmol) in toluene was added, and the reaction stirred at ambient temperature for 3 days. The reaction mixture was quenched with water and extracted three times with diethyl ether. The combined organic layers were washed with brine, dried with MgSO4, filtered, and concentrated. The residue was chromatographed on an AnaLogix SF25-60 g column and eluted with 10% EtOAc in hexanes to give Example 116A (0.88 g, 3.89 mmol, 64.8% yield). MS (DCI+): m/z 227.2 (M+H), 244.1 (M+NH4). 1H NMR (300 MHz, DMSO-d6) delta 8.93 (d, J=5.0 Hz, 1H), 7.96-7.90 (m, 1H), 7.82 (ddd, J=5.1, 1.5, 0.7 Hz, 1H), 2.90-2.68 (m, 4H), 2.35-2.21 (m, 1H), 2.13-2.00 (m, 1H).

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

Application of 622-75-3, 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. 622-75-3, name is 2,2′-(1,4-Phenylene)diacetonitrile, This compound has unique chemical properties. The synthetic route is as follows.

1,4-Benzene diacetonitrile solid (0.312 g, 2 mmol) and pyridine-4-carbaldehyde liquid (0.45 mL, 4.4 mmol) were added to a round bottom flask containing dichloromethane (40 mL). When the solid is completely dissolved, the solution is brownish yellow. The mixture was heated and stirred at 50 C in a water bath, and 0.45 mL of tetrabutylammonium hydroxide (TBAH, 40% methanol solution) was added by a syringe, and the solution was changed from brownish yellow to dark green. The reaction was stirred with a water bath at 50 C for 2 h, and TLC showed the reaction was completed. The solvent was evaporated to dryness with a rotary evaporator, and the solid was washed with water, filtered, and filtered, and then filtered, and then filtered and washed with EtOAc. The solid was 0.49 g. The yield was 73.5%.

The chemical industry reduces the impact on the environment during synthesis 2,2′-(1,4-Phenylene)diacetonitrile. I believe this compound will play a more active role in future production and life.