Category: nitriles-buliding-blocks

Reference of 5332-06-9, The chemical industry reduces the impact on the environment during synthesis 5332-06-9, name is 4-Bromobutanenitrile, I believe this compound will play a more active role in future production and life.

Piperidine (3 equiv.) and toluene (5.5 volumes based on 4-bromobutanenitrile weight) were mixed and heated to 55-60 C. To this mixture, 4-bromobutanenitrile (1 equiv.) was added slowly while keeping temperature below 80 C. Note the addition is exothermic and the exotherm is addition-controlled. A white solid was observed to crystallize during the addition (piperidine hydrobromide). After complete addition, the reaction was stirred at 55-60 C. for an additional 1 hour. Progress of the reaction was monitored by 1H NMR in CDCl3 by sampling from the slurry, filtering, and evaporating solvent. After reaction is finished, the mixture was cooled to 10-20 C. and stirred for 1 hour. Solids were removed by filtration, and the cake washed with toluene (2×1.5 volumes based on 4-bromobutanenitrile weight). The combined filtrates were evaporated under vacuum (15-50 mmHg) at 40-50 C. until 120-200% of the theoretical weight was obtained. The solution was again filtered to remove remaining piperidine hydrobromide solids. The filtrate was then further evaporated under vacuum (15-50 mmHg) at 40-50 C. until no more solvent distilled. 1H NMR in CDCl3 was done to quantify residual amount of toluene for correction in next step and to verify that there was no residual piperidine present.

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

455-18-5, name is 4-(Trifluoromethyl)benzonitrile, 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. Formula: C8H4F3N

Step A (4-Trifluoromethylphenyl)thiocarboxamide To a stirred solution of 25.0 grams (0.146 mole) of 4-(trifluoromethyl)benzonitrile in 190 ml of pyridine was added 14.8 grams (0.146 mole) of triethylamine. During a two hour period, hydrogen sulfide gas was bubbled into the reaction mixture. The reaction mixture was stirred under a dry nitrogen atmosphere for 15 minutes and then was poured into ice-water. The aqueous mixture was extracted with three portions of diethyl ether. The organic extracts were combined and washed in succession with 10% hydrochloric acid, water, and an aqueous, saturated sodium chloride solution. The washed extract was dried over anhydrous sodium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 28.3 grams of (4-trifluoromethylphenyl)thiocarboxamide as a solid.

The synthetic route of 455-18-5 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 3215-64-3, 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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of 15.3 g (100 mmol) of 2-(2,6difluorophenyl)acetonitrile, 152.5 g (70 mL, 812 mmol) of dibromoethane, and 32.7 g (144 mmol) of Et3BnN+Cl- was isolated from moisture and carbon dioxide and vigorously stirred at 60. A solution prepared from 95 g (1430 mmol, ?84.5%) of KOH and 95 mL of water was then added dropwise; the mixture was stirred during 6 h at 60-65C, and left overnight. On the next day, the reaction mixture was extracted with t-BuOMe (3×100 mL), the combined organic fractions were evaporated, and residual water was removed via azeotropic distillation with toluene. Then 60 mL of water and 40 mL of concentrated sulfuric acid were added to the obtained 1-(2,6-difluorophenyl)cyclopropanecarbonitrile, and the mixture was refluxed during 4 h. The reaction mass was cooled to ambient; the precipitate was filtered off and dried. Yield 17.82 g (90%), mp 156-157 (toluene).

The synthetic route of 2-(2,6-Dichlorophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

Related Products of 6575-12-8, A common heterocyclic compound, 6575-12-8, name is 2,6-Dibromobenzonitrile, molecular formula is C7H3Br2N, 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.

Embodiment 14 (S,E)-3-(4-((2-Hydroxymethylpyrrolidin-1-yl)methyl)-3,5-dimethoxystyryl)b iphenyl-2-carbonitrile 14 Synthesis of compound 14-c Phenylboronic acid (363mg, 3mmol) and 2,6-dibromobenzonitrile (783mg, 3mmol) were dissolved in a mixed solvent of 1,4-dioxane (20mL) and water (4mL), followed by addition of [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride dichloromethane complex (171mg, 0.21mmol) and sodium carbonate (1.06g, 10mmol). After the reaction system was purged three times with nitrogen, the reaction solution was heated to 80C and stirred for 16 hours. Then the reaction solution was cooled to room temperature and evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether) to give compound 14-c (280mg, yield 36%).

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. 17417-09-3, name is 2-Fluoro-5-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 2-Fluoro-5-nitrobenzonitrile

A solution of 2-fluoro-5-nitro-bezonitrile (300 mg, 1.81 mmol) and methyl hydrazine (170 mg, 3.62 mmol) in dioxane (10 mL) was stirred at 80 C. for 2 h. The reaction mixture was cooled and partitioned between 1N aqueous HCl and EtOAc. The organic layer was washed with water dried over Na2SO4 filtered and concentrated to the desired product 5-nitro-1-methyl-1H-indazol-3-ylamine (280 mg, 80%). HRMS for C8H8N4O2 (M+H) calcd: 193.0720. Found:193.0720

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.

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. 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8Cl4N2

Under nitrogen gas, 4,5-dichlorophthalonitrile (5.0 mmol), Ethyl vanillate (7.5 mmol), K2CO3 (50.0 mmol) was dissolved in 30 ml of anhydrous DMF and refluxed at 100 for 12 hours. When the reaction was complete, the reaction solution was slowly dropped on ice-water in a dropwise manner. The precipitate was filtered off under reduced pressure, washed with distilled water, and the dried crude product was purified by column chromatography (eluent: MC: MeOH = 15: 1)

According to the analysis of related databases, 1953-99-7, the application of this compound in the production field has become more and more popular.

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. 36282-26-5, name is 2-Bromo-4-fluorobenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C7H3BrFN

4-Fluoro-2-(2-oxooxazolidin-3-yl)bejizonitrile. A 48 mL pressure vessel containing 2-bromo-4-fluorobenzonitrile (1.00 g, 5.00 mmol), 2-oxazolidone (0.390 g, 4.50 mmol), K2CO3 (0.970 g, 7.0 mmol) and xantphos (0.231 g, 0.40 mmol) in dioxane (10 mL) was degassed with argon for 15 min. Pd2dba3 (0.140 g, 0.15 mmol) was introduced and then the reaction mixture was heated at 70 0C for 18 h. The mixture was cooled, diluted with dioxane, and then filtered through Celite. The resulting mixture was concentrated in vacuo and subjected to column chromatography on silica gel with hexanes-.ethyl acetate (1:1) to (3:7) gradient as the eluent to afford the title compound as a white solid (0.460 g, 50% yield): 1H NMR (400 MHz, CDCl3) delta ppm: 7.73 (IH, dd, J = 5.8, 8.6 Hz), 7.43 (IH, dd, J = 2.5, 9.6 Hz), 7.11 (IH, ddd, J = 2.5, 7.5, 8.7 Hz), 4.60 (2H, t, J = 7.1 Hz), 4.29 (2H, t, J = 7.1 HJz); LCMS f ESI, M+H*) m/z 207.

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.

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. 31643-49-9, name is 4-Nitrophthalonitrile, This compound has unique chemical properties. The synthetic route is as follows., category: nitriles-buliding-blocks

General procedure: 4-Nitrophthalonitrile (1mmol) 1, hydroxy compound (2mmol) 2 or 7 and dry potassium carbonate (8mmol) were dissolved in 50mL dry DMSO and stirred at room temperature under nitrogen for 48h. The reaction mixture was poured into 200mL distilled water and stirred for 15min. The crude product was recovered by filtration and washed with water. The residue was recrystallized from methanol/water mixture 1:1 and dried under vacuum.

According to the analysis of related databases, 31643-49-9, the application of this compound in the production field has become more and more popular.

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. 75344-77-3, name is 4-Bromo-3,5-dimethylbenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-3,5-dimethylbenzonitrile

Example 2; Preparation of (S)-2-tert-Butoxvcarbonvlamino-3-(4-cvano-2,6-dimethvl- phenvD-propionic acid methyl esterA 5OmL three-necked round bottom flask equipped with an addition funnel, magnetic stirrer, heating mantel, and thermocouple was charged under nitrogen dry DMAc (2mL), I2 (38.1 mg, 0.15mmol) and zinc powder activated (washed with 10% HCI, rinsed with H2O and acetone) (393 mg, 6 mmol). The resulting mixture was stirred at 23C until the red color of I2 disappeared (2 minutes). A solution of Boc-beta-iodo-L-alanine methyl ester (1 g, 3mmol) in DMAc (2 ml.) was added slowly, (temperature change from 210C to 29C) and the resulting mixture was stirred at 8O0C for 0.5-1 hour, then co cooled to 35C. To the resulting mixture were added, successively, 4-bromo-3,5-dimethyl- benzonithle (315 mg, 1.5mmol) in DMAc (6ml_), P(o-tol)3 (36.5 mg, 0.12 mmol) and Pd2(dba)3 (55 mg, O.Odeltammol). The resulting mixture was heated to 700C, with stirring for 1 hour, then cooled to ambient temperature. The resulting mixture was diluted with EtOAc (15ml_) and filtered with STAND SUPER-CEL 815520. The EtOAc solution was quenched with 1 N HCI (4OmL) and extracted with ethyl acetate (2OmL). The combined organic phases were washed with H2O (2 x 5OmL) and then with 50% brine, dried over Na2SO4 , filtered and evaporated to dryness in vacuo to yield a brown solid. The title compound was crystallized from EtOAc (5mL) and heptane (4OmL) to yield a white solid.

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 110882-60-5, 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. 110882-60-5 name is 3-Fluoro-5-nitrobenzonitrile, 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.

EXAMPLE 1; Step 2 To solution of 1.0 eq 1B in dry Et2O (0.06 M) at 0 C. was added dropwise a solution of diisobutyllithiumaluminum hydride (1.1 eq, 1.0 M in hexanes) by syringe. The resulting solution was kept at 0 C. 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.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Fluoro-5-nitrobenzonitrile, and friends who are interested can also refer to it.