Month: May 2021

Synthetic Route of 218632-01-0, 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. 218632-01-0, name is 3-Fluoro-4-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 3-fluoro-4-nitrobenzonitrile (200 mg, 1.2 mmol) in THF (2 mL) under an inert atmosphere was added 2,2,2-trifluoroethan-1-amine (0.11 mL, 1.44 mmol) and diisopropylethylamine (0.45 mL, 2.4 mmol) at room temperature. The reaction mixture was stirred at 100 C. for 16 h. After consumption of starting material (by TLC), the reaction mixture was diluted with water (20 mL) and extracted with EtOAc (2*20 mL). The combined organic extracts were washed with water (20 mL), dried over anhydrous Na2SO4 and concentrated under reduced pressure. The crude material was purified by silica gel column chromatography (eluent: 15-20% EtOAc/hexane) to afford 4-nitro-3-((2,2,2-trifluoroethyl amino)benzonitrile (260 mg, 1.09 mmol, 88%) as yellow solid. 1H NMR (400 MHz, DMSO-d6): delta 8.35-8.27 (m, 1H), 8.22 (d, J=8.7 Hz, 1H), 7.91 (s, 1H), 7.19 (dd, J=8.7, 1.5 Hz, 1H), 4.46-4.33 (m, 2H)

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

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. 1194-65-6, name is 2,6-Dichlorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: nitriles-buliding-blocks

In a 500 ml reaction flask, 51.6 g (0.3 mol) of 2,6-dichlorobenzonitrile, 41.6 g of water, and 0.6 g of a 30% sodium hydroxide solution were added.The temperature was raised to 35 C, and 55.65 g (0.45 mol) of 27.5% hydrogen peroxide was added dropwise.After 5 hours, the addition is completed.After the completion of the dropwise addition, the sample was controlled, and 2,6-dichlorobenzonitrile was ?0.5% qualified. Filtered, the filter cake was rinsed with 83.2 g of water.The wet product is dried to obtain 2,6-dichlorobenzamide 55g.The purity was >99.0%, and the yield was 97%.

The synthetic route of 1194-65-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 50670-64-9,Some common heterocyclic compound, 50670-64-9, name is 5-Amino-2-methylbenzonitrile, molecular formula is C8H8N2, 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 stirred solution of 3-((4-(1,8-naphthyridin-2-yl)phenoxy)methyl)benzoic acid (8) (100 mg, 0.28 mmol)in dimethyl formamide (2 mL), tetrahydrofuran (2 mL)was added corresponding anilines R-NH2 (9a-9k) (0.42mmol), 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride (0.42 mmol) and 4-dimethylaminopyridine(0.02 mmol) at room temperature and stirred at room temperature for 16 h. The reaction mixture was poured into ice water (4 mL) and extracted with ethyl acetate (3× 5 mL). The combined organic layers were washed with water (5 mL) followed by brine solution (5 mL), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure, crude material was washed with 50% of dichloromethane in pet ether to afford the pure compounds(10a-10k). Yields of the products varied between 40 and 75%.

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

Related Products of 1953-99-7,Some common heterocyclic compound, 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, molecular formula is C8Cl4N2, 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.

Five grams of 3,4,5,6-tetrachlorophthalonitrile, 3.06 grams of 2,6-dichlorophenol, 3.9 grams of K2CO3, and 25 milliliters of acetone were placed in a 100-milliliter flask and then Stir while heating at 70 °C. When the reaction was completed, the resultant was filtered and washed with acetone, and the resulting liquid was distilled to obtain a solid. Here, the obtained solid was dissolved in a small amount of dichloromethane and then washed with hexane several times, filtered and dried under vacuum to obtain 3,4,6-dichloro-5- (2,6-bis Chloro-phenoxy) -phthalonitrile.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, its application will become more common.

Electric Literature of 52133-67-2, 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. 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of the intermediate from Step A (1.01 g, 5.29 mmol) and NaOEt (0.72 g, 10.6 mmol) in EtOH (20 mL) was stirred at RT for 20 min. A solution of ethyl 2-cyano-4,4-diethoxybutanoate (1.34 g, 5.82 mmol) in 20 mL of EtOH was added and the resulting mixture was refluxed for 18 h. The reaction mixture was cooled to RT, concentrated in vacuo and the residue was diluted with EtOAc. The solution was then washed with water, dried over MgS04, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography using a 0percent to 15percent MeOH (with 2M NH3) in DCM gradient to give the title compound.

The chemical industry reduces the impact on the environment during synthesis Ethyl 2-cyano-4,4-diethoxybutyrate. I believe this compound will play a more active role in future production and life.

Electric Literature of 31643-49-9, A common heterocyclic compound, 31643-49-9, name is 4-Nitrophthalonitrile, molecular formula is C8H3N3O2, 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.

Propargyl alcohol (0.26 mL, 4.33 mmol) was added into a stirred mixture of 4-nitrophthalonitrile (0.50 g, 2.89 mmol) and anhydrous potassium carbonate (3.19 g, 23.1 mmol) in DMSO (6 cm3) under an argon atmosphere at room temperature. The mixture was stirred at room temperature for three and a half hour under an argon atmosphere, and then distilled to remove DMSO under reduced pressure. Water (100 cm3) was added to the dried mixture, which was then extracted with DCM. The organic layer was dried over MgSO4, and then the solvent was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with ethyl acetate/hexane to afford 3 as a solid (0.49 g, 85% chemical yield). 1H NMR (400 MHz, CDCl3) delta: 2.57 (t, J = 2.4 Hz, 1H), 4.75 (d, J = 2.4 Hz, 2H), 7.25 (dd, J = 8.8, J = 2.6 Hz, 1H), 7.31 (d, J = 2.6 Hz, 1H), 7.69 (d, J = 8.8 Hz, 1H). 13C NMR (100 MHz, CDCl3) delta: 56.6, 76.2, 77.8, 108.2, 115.2, 115.5, 117.4, 119.9, 120.2, 135.2, 160.5. Anal. Calc. for C, 72.52; H, 3.32; N, 15.38. Found: C, 71.94; H, 3.42; N, 15.48%.

The synthetic route of 31643-49-9 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 98730-77-9, name is 1-(Hydroxymethyl)cyclopropanecarbonitrile, molecular formula is C5H7NO, 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. Application In Synthesis of 1-(Hydroxymethyl)cyclopropanecarbonitrile

4-(3-(3-Fluoro-4-hydroxyphenyl)-4,4-dimethyl-5-oxo-2-thioxoimidazolidin-1-yl)-2-(trifluoromethyl)benzonitrile 1e (100 mg, 0.24 mmol) was placed in a reaction flask, followed by addition of 1-(hydroxymethyl)cyclopropanecarbonitrile 39a (28 mg, 0.28 mmol, prepared by a well known method described in Bioorganic and Medicinal Chemistry Letters, 2009, 19(6), 1797-1801), 1,1′-(azodicarbonyl)dipiperidine (95 mg, 0.38 mmol), 10 mL of methylbenzene, and tri-n-butylphosphine (76 mg, 0.38 mmol), successively. The reaction solution was warmed up to 50 C. and stirred for 12 hours. The reaction solution was concentrated under reduced pressure, and the resulting residue was purified by thin layer chromatography with elution system A to obtain the title compound 4-(3-(4-((1-cyanocyclopropyl)methoxy)-3-fluorophenyl)-4,4-dimethyl-5-oxo-2-thioxoimidazolidin-1-yl)-2-(trifluoromethyl)benzonitrile 39 (110 mg, yield 93.2%) as a white solid. MS m/z (ESI): 503.3 [M+1]; 1H NMR (400 MHz, CDCl3): delta 7.95-8.00 (m, 2H), 7.84 (d, 1H), 7.04-7.11 (m, 3H), 4.12 (s, 2H), 1.59 (s, 6H), 1.45 (t, 2H), 1.18 (t, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 98730-77-9, 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. 5332-06-9, name is 4-Bromobutanenitrile, This compound has unique chemical properties. The synthetic route is as follows., category: nitriles-buliding-blocks

To a stirred solution of 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine20 (11) (1.36 g, 6.6 mmol) and 4-bromobutyronitrile (0.98 g, 6.6 mmol) in DMF (40 mL), NaI (1.00 g, 6.6 mmol) and K2CO3 (2.75 g, 19.9 mmol) were added and the mixture was stirred at 60 C overnight. The solvent was removed under reduced pressure and the residue was diluted with H2O (150 mL) and extracted with ethyl acetate (3 × 100 mL) to give 4-(7,8-dimethoxy-4,5-dihydro-1H-benzo[d]azepin-3(2H)-yl)butanenitrile (1.66 g, 92%) as a yellow oil. 1H NMR (CDCl3) d: 6.64 (s, 2H), 3.85 (s, 6H), 2.86-2.82 (m, 4H), 2.63-2.59 (m, 4H), 2.58 (t, J = 6.8 Hz, 2H), 2.47 (t, J = 6.8 Hz, 2H), 1.84 (tt, J = 6.9 Hz, 6.9 Hz, 2H). This material (1.58 g, 5.7 mmol) was used without further purification and dissolved in dry THF (20 mL) for the following reaction. A solution of LiAlH4 (0.65 g, 17.1 mmol) in dry THF (20 mL) was added dropwise at 0 C. The mixture was stirred at rt overnight under N2. The mixture was cooled to 0 C and quenched by adding H2O (1 mL), 10% aqueous NaOH (2 mL), and H2O (2.5 mL) successively. The inorganic salts were washed with EtOAc and filtered. The filtrate was evaporated under reduced pressure to give 12 (1.18 g, 75%) as yellow oil. 1H NMR (CDCl3) d: 6.64 (s, 2H), 3.85 (s, 6H), 2.87-2.83 (m, 4H), 2.72 (t, J = 6.9 Hz, 2H), 2.64-2.60 (m, 4H), 2.48 (t, J = 6.9 Hz, 2H), 1.57-1.45 (m, 4H).

According to the analysis of related databases, 5332-06-9, the application of this compound in the production field has become more and more popular.

Some common heterocyclic compound, 60899-34-5, name is 1-Oxo-2,3-dihydro-1H-indene-4-carbonitrile, molecular formula is C10H7NO, 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. Application In Synthesis of 1-Oxo-2,3-dihydro-1H-indene-4-carbonitrile

To l-oxo-2,3-dihydro-7H-indene-4-carbonitrile INT-1 (42.5 g, 0.27 mol) and (i?)-2-methylpropane-2-sulfinamide (36.0 g, 0.30 mol) in toluene (530 mL) was added titanium tetraethoxide (84.1 mL, 92.5 g, 0.40 mol) and the reaction mixture was heated at 60C for 12 h under N2. The crude (i?)-N-(4-cyano-2,3-dihydro-lH- indene-l-ylidene)-2-methylpropane-2-sulfinamide INT-4 was used directly in the next experiment. LCMS-ESI (m/z) calculated for Ci4Hi6N2OS: 260.3; found 261.1 [M+H]+, = 3.19 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 60899-34-5, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 33279-01-5, name is 3-Oxopentanenitrile, 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 33279-01-5, Formula: C5H7NO

A mixture of a portion (0.6 g) of the material so obtained, hydrazine hydrate (0.28 ml) and ethanol (45 ml) was heated at 700C for 12 hours. The solvent was evaporated and the residue was purified by column chromatography on silica using a 19:1 mixture of methylene chloride and methanol as eluent. There was thus obtained the required starting material in 51% yield; 1H NMR: (DMSOd6) 1.04 (t, 3H), 2.41 (q, 2H), 4.4 (br s, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Oxopentanenitrile, and friends who are interested can also refer to it.