Author: Jessica.F

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.

Adding a certain compound to certain chemical reactions, such as: 110882-60-5, name is 3-Fluoro-5-nitrobenzonitrile, 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 110882-60-5, Recommanded Product: 3-Fluoro-5-nitrobenzonitrile

Example 1 Step 2. To solution of 1.0 eq IB in dry Et2O (0.06 M) at 00C was added dropwise a solution of diisobutyllithiumaluminum hydride (1.1 eq, 1.0 M in hexanes) by syringe. The resulting solution was kept at 00C overnight. The reaction mixture was added to a mixture of ice and glacial acetic acid. The reaction mixture was then diluted with ethyl acetate, and the aqueous layer was extracted with ethyl acetate two additional times. The combined organic layers were washed twice with saturated sodium bicarbonate, and once with brine. The organic layers were then dried over sodium sulfate, filtered and concentrated in vacuo. Purification over silica gel using 10% EtOAc/hexanes as the eluant afforded a yellow solid (100%) as an 80:20 mixture of 1C:1B. Example 1 Step 3. To cooled (00C) slurry of an 80:20 mixture of 1C:1B (1.0 eq) and boc-piperazine(about 2 eq) in a mixture of HOAc and DCM (4.8 M boc-piperazine in 1:1.4 v/v HOAc/DCM) was added sodium triacetoxyborohydride as a solid over about 5 minutes. The reaction was allowed to warm to RT and stirred for two hours. The reaction mixture was quenched with saturated sodium bicarbonate and diluted with ethyl acetate. The layers were separated and the aqueous layer was washed three times with ethyl acetate. The organic layers were combined and washed with brine, dried over sodium sulfate, and concentrated in vacuo. Purification by chromatography over silica gel using 50% ethyl acetate/hexanes as the eluant provided ID (67.7%) as a yellow oil.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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. 1023971-89-2, name is 2-Bromo-6-fluoro-4-methylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 1023971-89-2

Example 150A 4-Bromo-6-methyl-1H-indazol-3-amine 2-Bromo-6-fluoro-4-methylbenzonitrile (4.26 g, 19.9 mmol) was dissolved in ethanol (100 mL) and treated with hydrazine hydrate (3.99 g, 79.6 mmol). After stirring at reflux for 4 h, the mixture was cooled to RT and concentrated in vacuo. The residue was dissolved in a mixture of water and ethyl acetate. The aqueous layer was extracted once more with ethyl acetate. The combined organic layers were washed with water and with brine, dried over magnesium sulfate, concentrated in vacuo and dried to yield the title compound (4.40 g, 41% of theory) in a purity of 42%. LC-MS (Method 1B): Rt=0.72 min, MS (ESIPos): m/z=226 [M+H]+

According to the analysis of related databases, 1023971-89-2, the application of this compound in the production field has become more and more popular.

Application of 2920-38-9,Some common heterocyclic compound, 2920-38-9, name is [1,1′-Biphenyl]-4-carbonitrile, molecular formula is C13H9N, 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 the reaction vessel was added 30mol% CuCl, the reaction tube was evacuated, filled with oxygen,In an oxygen atmosphere, 0.2 mmol of p-phenylbenzonitrile, 0.6 mmol of ammonium chloride, 1 ml of acetonitrile and 1 ml of N, N-dimethylformamide were added, the reaction vessel was sealed, and reacted at 25 C,After the reaction is completed, it is washed with water, extracted with ethyl acetate, dried and concentrated by evaporation under reduced pressure to remove the solvent. The crude product is separated by column chromatography to obtain the desired product in a yield of 70%.

The synthetic route of 2920-38-9 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. 1009-35-4, name is 4-Fluoro-3-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 4-Fluoro-3-nitrobenzonitrile

Potassium hexamethyldisilazane [0.5 M in toluene] (12.04 mL, 24.08 mmol) was added to a solution of isopropanol (0.921 mL, 12.04 mmol) in tetrahydrofuran (20 mL) at 0° C. and stirred for 10 minutes. The resulting solution was added dropwise to a solution of commercially available 4-fluoro-3-nitrobenzonitrile at room temperature and stirred for several hours. Water was added and the product was extracted with ethyl acetate, dried with sodium sulfate and evaporated in vacuo to give the title compound

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.

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. 868-54-2, name is 2-Aminoprop-1-ene-1,1,3-tricarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 868-54-2

A 10% aqueous solution of KOH (5.60 ml, 10 mmol) andbenzyl chloride (1.15 ml, 10 mmol) were added consecutivelyto a stirred solution of of malononitrile dimer 1 (1.32 g,10 mmol) in DMF (20 ml). The mixture was stirred for 4 hat 20C and diluted with an equal volume of H2O. Theformed precipitate was filtered off, washed with H2O,EtOH, and hexane. Yield 1.80g (81%), colorless crystals,mp 140-142 (Et). IR spectrum, , cm-1: 3397-3295(N), 2219 (C?N). 1H NMR spectrum, delta, ppm (J, Hz):3.21 (1, dd, J = 7.8, J = 13.4) and 3.33 (1, dd, J = 8.6,J = 13.4, 2Ph); 4.18 (1, t, J = 8.0, CHCN); 7.27-7.36(5, m, H Ph); 8.80 (1, br. s) and 9.03 (1, br. s, NH2).Mass spectrum, m/z (Irel, %): 221 [M-]+ (100). Found, %:C 70.33; H 4.58; N 25.09. C13H10N4. Calculated, %:C 70.26; H 4.54; N 25.21.

The synthetic route of 868-54-2 has been constantly updated, and we look forward to future research findings.