Month: May 2021

Adding a certain compound to certain chemical reactions, such as: 77429-04-0, name is Ethyl 3-chloro-2-cyano-4,4,4-trifluorobut-2-enoate, 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 77429-04-0, HPLC of Formula: C7H5ClF3NO2

To a mixture of 21 g of ethyl 3-chloro-2-cyano-4,4,4-trifluorobut-2-enoate and 7.6 g of 4- nitrobenzimidamide in 300 ml of water, 31 ml of a aqueous sodium hydroxide solution (2M) were added. The reaction mixture was stirred at RT for 4 h, then diluted with 200 ml of water, acidified with half-concentrated aqueous hydrochloric acid to pH 3 and extracted with EtOAc (3 x 500 ml). The combined organic layers were dried over magnesium sulfate and the solvents were removed under reduced pressure. The crude product was purified by chromatography on silica gel eluting with a gradient of EtOAc/methanol. Yield: 2.7 g.

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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. 508203-48-3, name is 2,3-Difluoro-4-methylbenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 508203-48-3

To a suspension of 2,3-difluoro-4-methylbenzonitrile (5.0 g, 32.6 mmol) in ethanol (111 mL) at 25C was added hydroxylamine hydrochloride (4.5 g, 65.3 mmol). The reaction mixture was heated at80C for 2 h. After cooling to room temperature the volatiles were removed under reduced pressurethus affording a white solid that was used in the next step without purification.1H NMR (400 MHz, CDCI3) oe ppm: 7.30 (m, 1H), 6.95 (m, 1H), 6.50 (brs, 1H), 5.05 (brs, 2H),2.30 (s, 3H).

The synthetic route of 508203-48-3 has been constantly updated, and we look forward to future research findings.

Application of 159847-80-0, 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. 159847-80-0, name is Methyl 4-amino-3-cyanobenzoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-Amino-3-cyano-benzoic acid methyl ester (3.2 g, 10 mmol) in tetrahydrofurane/ water (110 ml, 1:1) was added lithium hydroxide hydrate (2.3 g, 30 mmol), the reaction mixture was stirred at room temperature for 20 hours and added hydro chloric acid (1 M) to pH = 3. From the mixture was tetrahydrofurane distilled of and the title compound precipitated out of solution.

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, Methyl 4-amino-3-cyanobenzoate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 220239-65-6,Some common heterocyclic compound, 220239-65-6, name is 4-fluoro-3-(trifluoromethyl)phenylacetonitrile, molecular formula is C9H5F4N, 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 H1 Preparation of 2-(4-fluoro-3-trifluoromethyl-phenyl)-ethylamine hydrochloride A solution of (4-fluoro-3-trifluoromethyl-phenyl)-acetonitrile (4.00 g, 19.3 mmol) in THF was added dropwise at 0-5 C. to a suspension of lithium aluminum hydride (1.61 g, 42.4 mmol) in diethyl ether (20 mL). The ice bath was removed and the reaction mixture was allowed to reach RT, then heated at reflux overnight. After cooling to 0 C., saturated aq. sodium sulfate solution was carefully added. After the initial exothermic reaction had subsided, the flask was allowed to warm to ambient temperature and solid magnesium sulfate (dry) was added to dry the suspension, which was subsequently filtered and washed with diethyl ether. After removal of the solvent, the residue was dissolved in diethyl ether (50 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 8 mL), and evaporated to dryness, leading to a solid orange foam. This residue was dissolved in dichloromethane (200 mL), and treated with water (100 mL), followed by 1 M aq. hydrochloric acid solution (50 mL), and stirred for 15 minutes, then the organic layer was separated and extracted a second time with 1 M aq. hydrochloric acid solution (50 mL). The combined aqueous phases were then washed with dichloromethane (50 mL), treated with concentrated aq. sodium hydroxide solution to adjust the pH to 12, and extracted twice with dichloromethane. The combined organic phases were washed with water and dried over magnesium sulfate. After filtration and evaporation of the solvent, the residue was dissolved in diethyl ether (5 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 2 mL), and stirred for 10 min. The precipitate was collected by filtration and dried to afford the title compound (632 mg, 13%). White solid, MS (ISP) 208.2 (M-Cl)+.

The synthetic route of 220239-65-6 has been constantly updated, and we look forward to future research findings.

Application of 1105665-42-6, These common heterocyclic compound, 1105665-42-6, name is 5-Bromo-2,3-difluorobenzonitrile, 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.

2,3-difluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile (0275) To a solution of 5-bromo-2,3-difluorobenzonitrile (140 mg, 0.64 mmol) in 1,4-dioxane (7 mL) were added 4,4,5,5-tetramethyl-2-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3,2-dioxaborolane (179.4 mg, 0.71 mmol), Pd(dppf)Cl2 (26.2 mg, 0.04 mmol) and potassium acetate (126 mg, 1.28 mmol) at room temperature. The resulting mixture was stirred for 2 h at 120 C. and then water (10 mL) was added. The mixture was extracted with ethyl acetate (30 mL×3). The organic phases were combined, washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to yield 2,3-difluoro-5-(tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile as brown oil (200 mg, crude). MS: m/z=266.0 [M+H]+.

The synthetic route of 1105665-42-6 has been constantly updated, and we look forward to future research findings.

Application of 57381-39-2, 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 57381-39-2 as follows.

EXAMPLE 6 4,2′-Difluoro-5′-(5-methyl-4-oxo-4,5-dihydroimidazo[4,5-c]pyridin-1-yl)biphenyl-2-carbonitrile 2-Bromo-5-fluorobenzonitrile was converted to 5-fluoro-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)benzonitrile as described in Example 2 to give a straw-coloured solid: deltaH (360 MHz, CDCl3) 1.38 (12H, s), 7.27 (1H, ddd, J 8, 8 and 2), 7.39 (1H, dd, J 9 and 2), 7.90 (1H, dd, J 8 and 6). 1-(3-Bromo-4-fluorophenyl)-5-methyl-1,5-dihydroimidazo[4,5-c]pyridin-4-one was coupled to 5-fluoro-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)benzonitrile, in the same way as in Example 1, to give 4,2′-difluoro-5′-(5-methyl-4-oxo-4,5-dihydroimidazo[4,5-c]pyridin-1-yl)biphenyl-2-carbonitrile as an off-white solid (360 mg, 55%): deltaH (400 MHz, d6-DMSO) 3.54 (3H, s), 6.67 (1H, d, J 7), 7.61 (1H, d, J 7), 7.69 (1H, t, J 9), 7.75-7.87 (4H, m), 8.09 (1H, dd, J 9 and 3), 8.38 (1H, s); m/z (ES+) 363 [MH+].

According to the analysis of related databases, 57381-39-2, the application of this compound in the production field has become more and more popular.

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. 4354-73-8, name is 2-Cyclohexylidenemalononitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 2-Cyclohexylidenemalononitrile

General procedure: Triethylamine, 1 mL, was added dropwise with stirring to a solution of 1.5 g (10 mmol) of cyclohexylidenemalononitrile and 10 mmol of substituted phenyl isothiocyanatein 2 mL of DMF. The mixture was stirred for 1 hat 50 C, cooled to room temperature, and diluted with 4 mL of methanol. The precipitate was filtered off, washed with water, and recrystallized from nitromethane. 3-Amino-2-phenyl-1-sulfanylidene-1,2,5,6,7,8-hexahydroisoquinoline-4-carbonitrile (1a) [12].Yield 2.252 g (78%), mp 270-271C. 1H NMR spectrum(DMSO-d6), delta, ppm: 1.75-1.81 m (4H, 6-H, 7-H),2.52-2.58 m (2H, 8-H), 2.67-2.73 m (2H, 5-H), 6.21 br.s (2H, NH2), 7.10-7.15 m (2H, Harom), 7.46-7.52 m (1H, Harom), 7.55-7.63 m (2H, Harom). 13C NMRspectrum (DMSO-d6), deltaC, ppm: 21.2, 22.4, 28.3, 28.5,78.6, 115.6, 126.5, 127.9, 128.8, 130.0, 138.7, 144.4,153.2, 181.9. Found, %: C 68.22; H 5.40; N 14.84;S 11.47. C16H15N3S. Calculated, %: C 68.30; H 5.37;N 14.93; S 11.40.

The synthetic route of 4354-73-8 has been constantly updated, and we look forward to future research findings.

Application of 72635-78-0, A common heterocyclic compound, 72635-78-0, name is 3-Amino-4-bromobenzonitrile, molecular formula is C7H5BrN2, 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.

To a mixture of 3-amino-4-bromo-benzonitrile (1.98 g, 10 mmol), TEA (5.06 g, 50 mmol), and methylene chloride (50 ml), mesyl chloride (2.71 ml, 35 mmol) was added at 0 C. and the mixture was stirred at room temperature for 30 min. Water was added to the reaction solution, which was then extracted with dichloromethane. The organic layer was dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were added with tetrahydrofuran (100 ml), water (400 mul) and sodium hydride (540 mg, 15.5 mmol), and stirred at room temperature for 16 hr. To the reaction solution, saturated aqueous solution of ammonium chloride (200 ml) was added followed by extraction with ethyl acetate. The organic layer was dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (2.48 g, 90%).1H-NMR (400 MHz, DMSO-d6) delta: 9. 82 (1H, s), 7. 87 (1H, d, J=4 Hz), 7. 75 (1H, d, J=8 Hz), 7. 70 (1H, dd, J=8 Hz, 4 Hz), 3. 14 (3H, s)HPLC retention time: 1.63 min (analysis condition U)

The synthetic route of 72635-78-0 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 2856-63-5, 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. 2856-63-5, name is 2-(2-Chlorophenyl)acetonitrile, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 30 Synthesis of 2-cyanomethylbiphenyl An oven dried resealable Schlenk tube was evacuated and backfilled with argon and charged with palladium acetate (2.2 mg, 0.01 mmol, 1.0 mol %), 2-(di-tert-butylphosphino)biphenyl (6.0 mg, 0.020 mmol, 2.0 mol %), phenylboron dihydroxide (183 mg. 1.5 mmol), and potassium fluoride (174 mg, 3.0 mmol). The tube was evacuated and backfilled with argon, and THF (1 mL) and 2-chlorobenzyl cyanide (152 mg, 1.0 mmol) were added through a rubber septum. The tube was sealed with a teflon screwcap, and the reaction mixture was stirred at room temperature until the starting aryl chloride had been completely consumed as judged by GC analysis. The reaction mixture was then diluted with ether (30 mL) and poured into a separatory funnel. The mixture was washed with 1.0 M NaOH (20 mL), and the aqueous layer was extracted with ether (20 mL). The combined organic layers were washed with brine (20 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated. The crude material was purified by flash chromatography on silica gel to afford 178 mg (92%) of the title compound.

The chemical industry reduces the impact on the environment during synthesis 2-(2-Chlorophenyl)acetonitrile. I believe this compound will play a more active role in future production and life.

Application of 10365-94-3, These common heterocyclic compound, 10365-94-3, name is 1,3,5-Benzenetricarbonitrile, 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.

Example 20:; Production of D-141:; D-141 was produced according to the following scheme:Production of D-141A:; 100 ml of methanol was added to 11.5 g of 1,3,5- tricyanobenzene produced in an ordinary manner, and then 26.0 ml of 50 % hydroxylamine solution was added to it, and stirred at 6O0C for 3 hours. After cooled, water was added to the reaction liquid, and the deposited crystal was taken out through filtration and dried to obtain 8.0 g of a crystal of D-141A.

Statistics shows that 1,3,5-Benzenetricarbonitrile is playing an increasingly important role. we look forward to future research findings about 10365-94-3.