Month: May 2021

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. 5414-21-1, name is 5-Bromovaleronitrile, A new synthetic method of this compound is introduced below., category: nitriles-buliding-blocks

General procedure: A solution of m-tolylmagnesium bromide 26, prepared from 416 muL of 3-bromotoluene and 83 mg of magnesium turnings in anhydrous THF (3 mL), was added dropwise under inert atmosphere to a solution of 5-bromovaleronitrile (400 muL, 3.43 mmol) in anhydrous THF (3 mL). The mixture was stirred at room temperature for 1 h, quenched with a saturated aqueous solution of NaHCO3 (3 mL) and extracted with dichloromethane (3 * 10 mL). The combined organic layers were dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude residue was purified by silica gel column chromatography (dichloromethane/methanol 95:5) to provide the compound 7 as a yellow oil (225 mg, 38% yield). Rf = 0.40 (dichloromethane/methanol 95:5). 1H NMR: delta 1.63-1.71 (m, 2H), 1.79-1.87 (m, 2H), 2.37 (s, 3H), 2.60-2.66 (m, 2H), 3.80-3.86 (m, 2H), 7.18-7.29 (m, 2H), 7.51-7.54 (m, 1H), 7.61-7.62 (m, 1H). 13C NMR: delta 20.0, 21.7, 22.1, 27.4, 50.1, 123.3, 126.8, 128.3, 130.5, 138.1, 140.4, 166.2. MS (ESI) m/z [M+H]+ Calcd for C12H16N+: 174.13. Found: 174.2.

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.

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. 53312-81-5, name is 5-Amino-2-fluorobenzonitrile, A new synthetic method of this compound is introduced below., Computed Properties of C7H5FN2

Compound 191 Triethylamine (0.206 mL, 0.00149 mol ) was added to a stirring mixture of 2-fluoro-6- methyl-3-[(3-methyloxetan-3-yl)sulfamoyl]benzoic acid (0.15 g, 0.000495 mol ) and CH3CN (10 mL ) under N2-atm. To the resulting solution was added HATU (0.207 g, 0.545 mmol). After stirring for 5 minutes, 5-amino-2-fluorobenzonitrile, (79.9 mg, 0.569 mmol ) was added, and the reaction mixture was stirred at room temperature for 20 hours. The reaction was next continued at 50C for 4 hours. The volatiles were evaporated and the obtained residue was dissolved in CH2CI2 (2.5 mL) and purified by silica gel Chromatography (heptane-EtOAc 100/0 to 0/100) followed by repurification with CH2Cl2-MeOH 100/0 to 98/2 as eluent. The desired fractions were combined and evaporated, and co-evaporated with EtOAc. The residue was dried further at 50C in vacuo, resulting in compound 191 (63 mg). Method F; Rt: 0.88 min. m/z: 420.1 (M-H)” Exact mass:421.1. 1H NMR (400 MHz, DMSO-d6) d ppm 1.46 (s, 3 H), 2.40 (s, 3 H), 4.19 (d, J=6.6 Hz, 2 H), 4.62 (d, J=6.2 Hz, 2 H), 7.36 (d, J=8.1 Hz, 1 H), 7.58 (t, J=9.1 Hz, 1 H), 7.80 (t, J=7.9 Hz, 1 H), 7.96 (ddd, J=9.1, 4.8, 2.8 Hz, 1 H), 8.22 (dd, J=5.7, 2.6 Hz, 1 H), 8.64 (s, 1 H), 11.16 (s, 1 H). 19F NMR (377 MHz, DMSO-de) delta ppm – 115.10 (d, J=7.9 Hz, 1 F), -113.61 (dt, J=8.9, 5.2 Hz, 1 F).

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.

Related Products of 868-54-2, A common heterocyclic compound, 868-54-2, name is 2-Aminoprop-1-ene-1,1,3-tricarbonitrile, molecular formula is C6H4N4, 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.

General procedure: Triethylamine (0.3 mmol) was added with stirring to an emulsion of salicylaldehyde 1 (3 mmol), 2-aminoprop-1-ene-1,1,3-tricarbonitrile (3 mmol, 0.40 g), and 2-pyrazolin-5-one 2 (3 mmol) in propanol or acetonitrile (2 mL). Then the mixture was stirred under reflux for 1 h, cooled, transferred onto a filter, washed with methanol (2 × 3 mL), and dried to isolate pure compound 3. In some cases, additional crystallization from DMSO was required.

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

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 1080-74-6 as follows. Formula: C12H6N2O

To a solution of intermediate 44 (255 mg, 0.15 mmol) in anhydrous chloroform (16 cm3) is added pyridine (0.85 cm3, 1 1 mmol). The mixture is then degassed with nitrogen before cooling to -40 C. 3- (Dicyanomethylidene)indan-l -one (205 mg, 1 .05 mmol) is added and the solution is further degassed for 10 minutes and with stirring, is allowed to warm before being held at -15 to -20 C. After 4 hours the reaction mixture is then added to methanol (100 cm3) washing in with methanol (2 x 10 cm3) and dichloromethane (10 cm3). Additional methanol (50 cm3) is added and the suspension stirred for 10 minutes before the solid is collected by vacuum filtration, washing the solid with additional methanol (3 x 10 cm3). The crude product is purified by silica plug (40-60 petrol:dichloromethane; 1 :4), concentrating the product in vacuo. The solid is then triturated with methanol (3 x 10 cm3) and collected by filtration, before being additionally washed with cyclohexane (3 x 10 cm3), diethyl ether (3 x 10 cm3), acetone (3 x 10 cm3), methyl ethyl ketone (10 cm3) and ethyl acetate (3 x 10 cm3) to give compound 103 (203 mg, 66%) as a partially pure black solid. 1H NMR (400 MHz, CDCIs) 9.58 (2H, s), 9.28 (2H, d, J 8.6), 8.74 (2H, d, J 7.8), 8.36 (2H, s), 7.93 – 8.00 (4H, m), 7.75 – 7.86 (4H, m), 7.23 – 7.27 (8H, m), 6.83 – 6.89 (8H, m), 3.92 (8H, t, J 6.5), 1 .70 – 1 .80 (8H, m), 1 .38 – 1 .46 (8H, m), 1 .18 – 1 .37 (64H, m), 0.87 (12H, t, J 6.9).

According to the analysis of related databases, 1080-74-6, the application of this compound in the production field has become more and more popular.

Related Products of 3672-47-7, A common heterocyclic compound, 3672-47-7, name is 3-(4-Methoxyphenyl)-3-oxopropanenitrile, molecular formula is C10H9NO2, 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.

General procedure: To a 0.5-2.0ml vial with 1 mmol ketone (1 eq) issolved in 2-pentanol (1.66 M) was added 1.1 eq of aromatic aldehyde and catalytic piperidine (0.08 eq), stirring vigorously. After heating under muWave for 15min at 120 C, the reaction was cooled to r.t. and precipitate was vacuum filtered and washed with minimal, cold hexanes. After drying under vacuum, solid was analyzed via NMR, IR, and mp.

The synthetic route of 3672-47-7 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 53312-82-6, name is 4-Amino-2-bromobenzonitrile, 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. Computed Properties of C7H5BrN2

To a mixture of 4-amino-2-bromobenzonitrile (1.00 g, 5.08 mmol), 2-ethyl-5,7-dimethyl- 3-(4-(4,4,5,5-tetramethyl-1 ,2-dioxaborolan-2-yl)benzyl)-3H-imidazo[4,5-b]pyridine (OOld, 1.773 g, 4.53 mmol) and K2C03 (2.505 g, 18.13 mmol) was added 1,4-dioxane and 0 (2:1, 30 mL). The reaction mixture was then purged with a stream of N2 for 5 min in a sealable vial before Pd(Ph3P)4 (0.262 g, 0.227 mmol) was added. The reaction vial was sealed and the mixture heated at 100C for 18h. The cooled reaction mixture was then diluted with EtOAc (50 mL), washed with 0 and brine, dried (Na2S04) and evaporated. The crude residue was purified by flash chromatography (ISCO, 0-100% EtOAc-DCM) to afford the title compound (1.46 g, 4.53 mmol, 85%) as a white solid. LC-MS (Method H): 1.220 min, [M + H]+= 382.5; H NMR (400 MHz, CDC13) delta ppm 7.37 – 7.55 (m, 3H), 7.19 (d, / = 8.2 Hz, 2H), 6.90 (s, 1H), 6.51 – 6.68 (m, 2H), 5.51 (s, 2H), 4.17 (br s, 2H), 2.81 (d, / = 7.4 Hz, 2H), 2.59 (s, 3H), 2.64 (s, 3H), 1.33 (t, / = 7.4 Hz, 3H).

The synthetic route of 4-Amino-2-bromobenzonitrile has been constantly updated, and we look forward to future research findings.

35704-19-9, name is N-(4-Cyanophenyl)acetamide, belongs to nitriles-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: nitriles-buliding-blocks

General procedure: A mixture of 1a (34 mg, 0.250 mmol), 2a (149 mg, 0.500 mmol) and TBAT (540 mg, 1.00 mmol) in toluene (3 mL) was stirred at 50 C for 18 h. After this time, the reaction mixture was cooled to ambient temperature and concentrated under reduced pressure. The residue obtained was purified by flash chromatography (silica, heptane to 2:3 ethyl acetate/heptane) to afford 3a (45 mg, 85%) as an off-white solid.

The synthetic route of 35704-19-9 has been constantly updated, and we look forward to future research findings.

Electric Literature of 17626-40-3,Some common heterocyclic compound, 17626-40-3, name is 3,4-Diaminobenzonitrile, molecular formula is C7H7N3, 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 stined solution of 3, 4-diammobenzanitrile (IC; 200 mg, 1.5 mmol) in THF (10 mL) under argon atmosphere was added carbonyl diimidazole (243 mg, 1.5 mmol) at RT and stirred for 16 h. The volatile were concentrated raider reduced pressure. The crude material was purified by silica gel column chromatography (eiuent: 40% Acetone Hexane) to afford compound ID (60 mg, 0.37 mmol, 24%) as an off-white solid. H NMR (400 MHz, DMSO- : delta 11.16 (b s; IH), 11.04 (br s, IH), 7.39 (dd, 7= 8. L 1.6 Hz, IH), 7.30 (s, IH), 7.06 (d, 7 = 8.2 Hz. IH).

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-Diaminobenzonitrile, its application will become more common.

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. 96784-54-2, name is 3-Methyl-4-nitrobenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C8H6N2O2

To a mixture of 3-methyl-4-nitrobenzonitrile (20g, 12.3 mmol), 3-trifluoromethyl-2,2,2- trifluoroacetophenone (33g, 13.6mmol) and i-Pr2NEt (32g, 24.6mmol) in 40m1 of THF was added TBAF (160g, 61.5 mmol) at room temperature. After the addition, the mixture was refluxed for 24h. Then, the reaction mixture was poured into water and extracted with ethyl acetate three times. The combined organic layers were dried over sodium sulfate, filtered and concentrated under vacuum. The residue was purified by column chromatography on silica gel to give the title compound (36 g, 80% yield). 1H NMR (300Mz, DMSO-d6): delta 3.90 (d, 1H), 4.13 (d, 1H), 7.32 (d, 1H), 7.75-7.79 (m, 3H), 7.88-7.90 (m, 1H), 7.93-8.00 (m, 2H).

The synthetic route of 96784-54-2 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 6136-68-1, The chemical industry reduces the impact on the environment during synthesis 6136-68-1, name is 3-Acetylbenzonitrile, I believe this compound will play a more active role in future production and life.

Part A. Preparation of ethyl 3-(3-cyanophenyl)-3-oxopropionate. To a suspension of sodium hydride (1.2 g of 60% suspension in mineral oil, hexane-washed, 30.3 mmol) in 40 mL of tetrahydrofuran was added diethyl carbonate (3.7 mL, 30.3 mmol) and 3-acetyl benzonitrile (2.2 g, 15.2 mmol). The resulting suspension was stirred at 65 C. for 1 h and then was cooled to room temperature. There was added 40 mL of 10% aqueous HCl and the reaction mixture was diluted with ethyl acetate and the layers were separated. The organic layer was washed with brine, dried (MgSO4) and concentrated in vacuo to afford 3.2 g (96%) of the title compound, which was sufficiently pure to be used without purification. MS (NH3-CI) 218.3 (M+H)+.

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-Acetylbenzonitrile, other downstream synthetic routes, hurry up and to see.