Author: Jessica.F

Synthetic Route of 64248-64-2, The chemical industry reduces the impact on the environment during synthesis 64248-64-2, name is 2,5-Difluorobenzonitrile, I believe this compound will play a more active role in future production and life.

Step A: 5-Fluoro-2-hydroxybenzonitrile (23t): 2,5-Difluorobenzonitrile (14.9 g, 107 mmol) and benzyl alcohol (11.1 mL, 11.6 g, 107 mmol) were dissolved in DMF (330 mL) and cooled to 0 C. Sodium hydride (60% in oil, 6.40 g, 161 mmol) was added to the solution at 0 C. and the reaction mixture was allowed to warm to room temperature. After stirring for 1 hour at room temperature, the reaction solution was cooled to 0 C. and water (330 mL) was gradually added to the solution. The mixture was transferred to a separatory funnel and extracted three times with 500 mL of Et2O. The combined organic layer was washed twice with 100 mL of water, brine once, then dried over MgSO4. After filtration, the solution was concentrated under reduced pressure to obtain a crude pale yellow solid. The crude solid was dissolved in MeOH (500 mL). To the solution was added 10% palladium on activated carbon under a nitrogen atmosphere. Replacing nitrogen gas with hydrogen gas, reaction mixture was stirred at room temperature (if the reaction did not proceed in 30 minutes, the Pd/C was filtered off and the reaction was set up again). After 2 hours of stirring, the palladium on carbon was filtrated off and washed with MeOH. The solution was concentrated under reduced pressure to obtain a pale yellow solid. The solid was recrystallized from hot toluene (100 mL) by addition of hexane (10 mL) followed by cooling to 0 C. The obtained white needles were washed with 1:1 mixture of toluene and hexane (7.23 g, 49% yield). Mother liquor was concentrated and purified on silica gel with Et2O/hexane (2:3-1:1) to afford the desired compound (23t) (6.94 g, 47% yield). Total 14.2 g (96% yield) over 2 steps. 1H-NMR (400 MHz, d6-DMSO) delta 11.09 (s, 1H), 7.58 (dd, J=8.4, 3.2 Hz, 1H), 7.40 (td, J=8.6, 3.2 Hz, 1H), 7.03 (dd, J=9.2,4.4 Hz, 1H) ppm.

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, 2,5-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 50670-64-9, name is 5-Amino-2-methylbenzonitrile, 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 50670-64-9, Formula: C8H8N2

To a stirred solution of 5-Amino-2-methylbenzonitrile (4.00 g, 30.27 mmol) in 33% sulfuric acid (45 mL) was added a solution of sodium nitrite (2.09 g, 30.27 mmol) in water (15 mL) at 5C. The temperature was kept below 5C. In a separated flask, concentrated sulfuric acid (30 mL) was added cautiously to a stirred solution of sodium sulfate (21.50 g, 151.33 mmol) in water (15 mL). The slurry was heated to reflux. The prepared diazonium salt was added dropwise to the refluxing mixture and the reflux was continued for 2 hours. The mixture was cooled slowly to room temperature. The mixture was extracted with ethyl acetate (2 x 100 mL) and the combined extracts were washed with water (2 x 150 mL). The organic layer was extracted with aqueous 10% NaOH solution (2 x 100 mL). The alkaline extract was acidified with cone. HC1 and extracted with EtOAc (2 x 100 mL). The combined organic layers were dried over MgSCL, filtered and the solvent was evaporated in vacuo to afford the title compound as a red solid and pure enough to be used as such (2400 mg, 60% yield). 1H NMR (300MHz, CHCL-d) 9.46 (bs, 1H), 7.16 (d, / = 8.4 Hz, 1H), 7.06 (d, / = 2.7 Hz, 1H), 6.97 (dd, / = 8.4 and 2.7 Hz, 1H ), 2.45 (s, 3H).

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, 5-Amino-2-methylbenzonitrile, other downstream synthetic routes, hurry up and to see.

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. 263159-64-4, name is 2-Bromo-3-methylbenzonitrile, A new synthetic method of this compound is introduced below., SDS of cas: 263159-64-4

Step 3: A mixture of compound 249 (1 1 g, 56.1 mmol), NBS (10 g, 56.1 mmol) and BPO (81 mg, 0.34 mmol) in CCI4 (150 mL) was heated at reflux overnight. TLC (petroleum ether / EtOAc = 5:1 ) showed the reaction was completed. The mixture was filtered and the filtrate was concentrated. The residue was purified by column chromatography over silica gel (petroleum ether / EtOAc = 20:1 ) to yield compound 250 (9.6 g, 62%) as a white solid. 1H NMR (400 MHz, CDCI3) delta 7.69- 7.67 (d, 1 H), 7.63-7.61 (d, 1 H), 7.45-7.41 (t, 1 H), 4.61 (s, 2H)

The synthetic route of 263159-64-4 has been constantly updated, and we look forward to future research findings.

Reference of 70591-86-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 70591-86-5 name is 3-Bromobenzoylacetonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A mixture of 3-(3-bromophenyl)-3-oxopropanenitrile (35 g, 156 mmol) and hydrazine hydrate (11.34 mL, 234 mmol) in ethanol (600 mL) was refluxed for 16 h. Mixture was then cooled and concentrated in vacuuo. Crude product was diluted with dichloromethane and stirred for 5 min. Solids were filtered and dried to afford 3-(3-bromophenyl)-1H-pyrazol-5-amine (30 g, 126 mmol, 81 % yield) as off-white solid. 1H NMR (400 MHz, DMSO-d6) delta 12.02 (br. s., 0.4H), 11.66 (br. s., 0.6H), 7.86 (t, J=1.6 Hz, 1H), 7.67 (d, J=7.5 Hz, 1H), 7.45 (d, J=6.8 Hz, 1H), 7.37 – 7.18 (m, 1H), 5.78 (br. s., 1H), 5.08 (br. s., 1.2H), 4.68 (br. s., 0.8H). LCMS (M+H) = 240.1.

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

Electric Literature of 4426-11-3, 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. 4426-11-3, name is Cyclobutanecarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 240A 1-[2-(trifluoromethyl)pyridin-4-yl]cyclobutanecarbonitrile A solution of cyclobutanecarbonitrile (1.36 g, 16.77 mmol) and 4-chloro-2-(trifluoromethyl)pyridine (2.89 g, 15.92 mmol) in anhydrous THF (55 mL) was chilled to -75 C. 1.0M lithium hexamethyl disilazide (24 mL, 24.00 mmol) in THF was added dropwise, and the reaction was permitted to warm to ambient temperature overnight. The reaction was quenched with saturated NH4Cl solution (200 mL) and extracted with EtOAc (300 mL). The organic layer was washed with saturated NH4Cl solution (200 mL), dried over Na2SO4, filtered, and concentrated. The residue was chromatographed on silica (5-50% EtOAc in heptane) to give Example 240A (2.162 g, 7.65 mmol, 48% yield) as an orange oil. LC/MS (APCI+): m/z 227 (M+H). 1H NMR (300 MHz, DMSO-d6) delta 8.84 (d, J=5.1 Hz, 1H), 8.00 (d, J=1.3 Hz, 1H), 7.90-7.82 (m, 1H), 2.89-2.66 (m, 4H), 2.42-2.22 (m, 1H), 2.13-1.90 (m, 1H).

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, Cyclobutanecarbonitrile, other downstream synthetic routes, hurry up and to see.

Reference of 261951-81-9, 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. 261951-81-9, name is 3-Fluoro-2-(trifluoromethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 3-fluoro-2- (trifluoromethyl)benzonitrile g, 6.3 mmol) and piperazine (0.72 g, 8,4 mmol) in acetonitrile (6 ml) was heated under microwave radiation at 150 C for 15 minutes. The reaction mixture was poured into water (50 ml) and the aqueous phase was extracted with ethylacetate (3×50 ml). The combined organic phases was dried (MgS04), filtered and evaporated to dryness. Purification by flash column chromatography (ethylacetate/methanol, 1:1) gave the title compound: 1.1 g. MS m/z (rel. intensity, 70 eV) 255 (M+, 16), 214 (11), 213 (bp), 171 (8), 151 (7).

The synthetic route of 3-Fluoro-2-(trifluoromethyl)benzonitrile 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. 3759-28-2, name is 2-(Cyanomethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 3759-28-2

General procedure: To a solution of homophthalonitrile 2 (129 mg, 0.82 mmol) in PriOH (4 ml), salicylaldehyde 1 (2.46 mmol) and NH4OAc (143 mg, 1.64 mmol) were added. The mixture was placed into a microwave reactor and heated at 150 C for 10 min. The vessel was opened, MeNO2 (0.439 ml, 8.2 mmol) and Et3N (0.114 ml, 0.82 mmol) were added, the mixture was heated again in the microwave reactor at 150 C for 10 min. The solvent was evaporated under reduced pressure, the residue was chromatographed on silica gel (EtOAc-hexane, 1:5-1:1) (method A) or was dissolved in asmall volume of Et2O or CH2Cl2 and extracted with HCl aqueous solution(0.6 m, 3 30 ml). The aqueous layer was neutralized with Na2CO3. The precipitate was filtered off and washed with H2O several times and once with a small amount (1.5 ml) of PriOH and dried in air (method B).

The synthetic route of 3759-28-2 has been constantly updated, and we look forward to future research findings.

Related Products of 7357-70-2, The chemical industry reduces the impact on the environment during synthesis 7357-70-2, name is 2-Cyanothioacetamide, I believe this compound will play a more active role in future production and life.

General procedure: Cyanothioacetamide (for X=S) (1.5 equiv) or cyanoacetamide (for X=O) (1.5 equiv) was added to a solution of the 1, 3-diones (for R4= -CF3 and -CH3) (1.0 equiv) or enaminones (for R4=H) (1.0 equiv) in ethanol in the presence of DABCO (1.0 equiv) at room temperature. The reaction mixture was stirred under reux for 3-6 h until complete conversion of the starting materials, as monitored by TLC. After cooled to room temperature, the solvent was evaporated under reduced pressure and the residue was neutralized with diluted hydrochloric acid (1 N) to precipitate the crude products. After filtrated and dried in vacuo, the product can be straight used for step d. Yield: 70-90%.

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

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. 874-97-5, name is 3-Cyanobenzyl alcohol, A new synthetic method of this compound is introduced below., Formula: C8H7NO

Preparation of 3-(iodomethyl)benzonitrile After 3-(hydroxymethyl)benzonitrile (1.33 g, 10 mmol) was dissolved in dimethylformamide (18 mL), triphenylphosphine (3.14 g, 12 mmol) and imidazole (0.82 g, 12 mmol) were added thereto, and the mixture was cooled to -20 C. Iodine (2.79 g, 11 mmol) was added dividing in 5 portions thereto, and the result was stirred for 2 hours at -10 C. A 5% aqueous ammonium chloride solution (60 mL) was added to the reaction solution, and the result was extracted with a diethyl ether/ethyl acetate=1/1 solution (60 mL*2). The organic layers were combined, washed with a 1% aqueous sodium thiosulfate solution to remove excess iodine, washed with salted water, dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was separated and purified using silica gel column chromatography (ethyl acetate/normal-hexane=1/9) to give a target compound (1.9 g, 78%) in a white powder state. 1H-NMR (300 MHz, CDCl3) delta 4.41 (s, 2H), 7.2-7.66 (m, 4H); MS (EI, m/e)=243 (M+).

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.

Synthetic Route of 90401-84-6, 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. 90401-84-6, name is 6-Cyano-1-tetralone belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 250 mL round bottom flask, (methoxymethyl) (triphenyl)phosphonium chloride (4.0 g, 12 mmol) was dissolved in THF (20 mL). The solution was cooled to -78 C. To above solution was added n-butyl lithium (3.50 mL, 2.50 M in Hexane, 8.8 mmol) dropwise. Reaction color changed to orange. The mixture was cooled to -78 C and to it was added 5-oxo-5,6,7,8-tetrahydronaphthalene-2-carbonitrile (1 g, 5.77 mmol). The reaction was let warm to RT and stirred at r.t for 18 hours. The reaction was then quenched with addition of saturated ammonium chloride (5 mL) and extracted with dichloromethane. The organic phase was washed with brine (5 mL), dried over anhydrous Na2SO4, filtered, concentrated and purified by flash column chromatography (Hexane/EtOAc 0-50%). The desired product was obtained. 1H NMR (500 MHz, CDCl3, delta in ppm): 7.0 -7.6 (3H, aromatic), 6.75 (1H, s), 3.88 (3H, s, Me), 3.0 (1H, t), 2.63 (2H, t), 2.23 (1H, t), 2.18 (1H, t), 1.65 (1H, t).

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, 6-Cyano-1-tetralone, other downstream synthetic routes, hurry up and to see.