Month: May 2021

Application of 185836-35-5, A common heterocyclic compound, 185836-35-5, name is 4-(Benzyloxy)-2-fluorobenzonitrile, molecular formula is C14H10FNO, 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.

5.1. 2-[[(1-Methylethylidene)amino]oxy]-4-(phenylmethoxy)benzonitrile A solution of 7.83 g (0.107 mol) of acetone oxime in 200 ml of dimethylformamide is stirred for 30 minutes in the presence of 12 g (0.11 mol) of 95% potassium t-butanolate. A solution of 20.3 g (0.089 mol) of 2-fluoro-4-(phenylmethoxy)benzonitrile in 100 ml of dimethylformamide is then added over 15 minutes. The mixture is stirred for 2 hours and then poured into ice-water. The crystalline product is filtered off and dissolved in dichloromethane, and the solution is then dried over sodium sulphate and concentrated under reduced pressure. 21.2 g of product are obtained. Melting point: 102 C.

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 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 4553-07-5 as follows. Formula: C11H11NO2

A slurry of sodium hydride (60% dispersion in mineral oil, 811 mg, 20.2 mmol) in dry THF (170 mL) at 0C was added with ethyl 2-cyano-2-phenylacetate (3.2 g, 16.9 mmol). The resulting mixture was stirred for one hour at 0C before adding methyl iodide (2.87 mL, 30.3 mmol) dropwise and slowly warming the mixture to roomtemperature over 16 hours. The mixture was then quenched with saturated aqueous NH4C1 (100 mL) and EtOAc (200 mL). The layers were separated and the aqueous phase was back-extracted with EtOAc (3 x 50 mL). The combined organic phases were dried (MgSO4), filtered and the solvent was removed in vacuo. The residue was purified by silica gel colunm chromatography, eluting with 10% EtOAc in isohexane to give the titlecompound as a colourless oil (2.2 g, 64%).?H NMR (400 MHz, CDC13): oe 7.55-7.5 1 (m, 2 H), 7.44-7.36 (m, 3 H), 4.26-4.22 (m, 2 H), 1.96 (s, 3 H), 1.25 (t, J = 7.2 Hz, 3 H).

According to the analysis of related databases, 4553-07-5, the application of this compound in the production field has become more and more popular.

Reference of 3759-28-2,Some common heterocyclic compound, 3759-28-2, name is 2-(Cyanomethyl)benzonitrile, molecular formula is C9H6N2, 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 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).

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

Application of 33279-01-5,Some common heterocyclic compound, 33279-01-5, name is 3-Oxopentanenitrile, 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.

To a solution of 3-oxopentanenitrile (0.74 g, 7.6 mmol) and quinolin-5-yl-hydrazine (prepared from Example 4 step a, 1.0 g, 6.3 mmol) in ethanol (5 mL) was heated at 80 C. for 3 h with stirring. After cooling to room temperature, 20% aqueous sodium hydroxide (1.5 mL) was added to the reaction mixture and then heated at 70 C. for 3 h. The reaction mixture was cooled to room temperature and concentrated in vacuo. The crude residue was dissolved in 1:1 dichloromethane/methanol (40 mL) and the phases were separated. The organic layer was dried (Na2SO4), and filtered through a pad of Celite. The filtrate was concentrated in vacuo and the crude residue was purified by flash chromatography (SiO2, 1-10% methanol containing 10% ammonium hydroxide in dichloromethane) to give the desired product (0.83 g, 3.5 mmol, 55%).

The synthetic route of 33279-01-5 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 116332-64-0, name is 4-Cyano-N-methoxy-N-methylbenzamide, 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 116332-64-0, Quality Control of 4-Cyano-N-methoxy-N-methylbenzamide

To a -780C stirred solution of trimethyl (2-methylbut-3-yn-2-yloxy) silane (3.3 g, 20.00 mmol) in dry THF (45 mL), «-BuLi (4.1 mL, 9.00 mmol, 1.6 M in hexane) was added dropwise over 10 minutes under an inert atmosphere. The reaction mixture was stirred for 30 min at -78 0C, and then a solution of 4-cyano-N-methoxy-N-methylbenzamide (2.0 g, 10.00 mmol) in dry THF (15 mL) was added to the reaction mixture and stirring was continued for an additional 1 h at -78 0C. The reaction mixture was quenched with a saturated NH4Cl solution and extracted with EtOAc (2 x 100 mL). The combined organic layers were washed with water (50 mL) and brine (50 mL), dried OVCr Na2SO4, filtered, and concentrated in vacuo to obtain the crude product. The crude material was purified via silica gel column chromatography eluting with 15 % EtOAc in hexanes to afford 4-(4- methyl-4-(trimethylsilyloxy) pent-2-ynoyl) benzonitrile (3.8 g, 68 %) as a yellow oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Cyano-N-methoxy-N-methylbenzamide, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 623-03-0, name is 4-Chlorobenzonitrile, 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 623-03-0, Recommanded Product: 4-Chlorobenzonitrile

General procedure: A two-necked 25.0mL flask fitted with a reflux condenser and septum was charged with aryl halide (1.0mmol), phenylboronic acid (1.2mmol), KOH (2.0mmol), diethyleneglycol-di-n-butylether (0.6mmol, internal standard), and the palladium-pyridine catalyst (0.01mol %) in isopropyl alcohol (1.0mL) was added. The mixture was heated to 82C under an air atmosphere. The conversion was monitored by gas chromatography.

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.

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. 149793-69-1, name is 3-Fluoro-5-(trifluoromethyl)benzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Fluoro-5-(trifluoromethyl)benzonitrile

Example-1: Preparation of 3-fluoro-5-(trifluoromethyl)benzamide : In 2 lit three necked round bottom flask equipped with mechanical stirrer, thermometer and an addition funnel, 3-fluoro-5(trifluoromethyl)benzonitrile (100 g) and dimethylsulfoxide (200 ml) was added at 25-35C and stirred for 20 min. To this, potassium carbonate (220 g) and hydrogen peroxide solution (140 ml) were added at 25-35C and stirred for 90 mins. After completion of reaction, water (1200 ml) was added to the reaction mass and stirred for an hour. Filtered the solid, washed with water, suck dried and then dried at 50-55C under vacuum for 6 hrs to get the title compound. Yield: 103 g.

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.

Adding a certain compound to certain chemical reactions, such as: 658-99-1, name is 2-(3,4-Difluorophenyl)acetonitrile, 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 658-99-1, name: 2-(3,4-Difluorophenyl)acetonitrile

77.1 Synthesis of 3-cyano-3-(3,4-difluoro-phenyl)-pentanedioic acid diethyl ester Prepare by the method of Example 11.1.2 using 3,4-difluorophenylacetonitrile to give the title compound.

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-(3,4-Difluorophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

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. 1194-02-1, name is 4-Fluorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 4-Fluorobenzonitrile

General procedure: To a solution of nitrile 6 (3.3 mmol, 1.0 equiv) in EtOH (15 mL) was added hydroxylamine hydrochloride (4.0 mmol, 1.2 equiv) and NaHCO3 (6.6 mmol, 2.0 equiv). The mixture was refluxed for 4 h. The reaction mixture was diluted with EtOAc, filtered, and concentrated in vacuo. Water was added to the residue and extracted with ethyl acetate (3 x 30 mL), washed with brine (1 x 30 mL), driedover anhydrous MgSO4, and concentrated. The residue was subjected to silica gel chromatography with EtOAc/MeOH (9:1) to make carboxamidine 7.

The synthetic route of 1194-02-1 has been constantly updated, and we look forward to future research findings.

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. 53312-81-5, name is 5-Amino-2-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 5-Amino-2-fluorobenzonitrile

Step 12: Preparation for 2-Fluoro-5-((5-isopropoxy-2,3-dihydro-[1,4]dioxino[2,3-f]quinazolin-10-yl)amino)benzonitrile To a solution of 10-chloro-5-isopropoxy-2,3-dihydro-[1,4]dioxino[2,3-f]quinazoline (0.05 g, 0.18 mmol) in isopropanol (3 mL) was added 4-chloro-3-nitroaniline (0.030 g, 0.20 mmol). The solution was stirred at 80 C. for 4 hours. After cooling to ambient temperature, the solution was concentrated to obtain a yellow solid which was purified by column chromatography on silicon gel (dichloromethane:methanol=100:1) to obtain a yellow solid (0.045 g, yield=55%). 1H NMR (DMSO-d6, 400 MHz): delta 10.54 (s, 1H), 8.76 (s, 1 Hz), 8.24-8.23 (m, 1H), 8.04 (t, 1H, J=8.8 Hz), 7.66 (t, 1H, J=8.8 Hz), 7.21 (s, 1H), 4.79 (dd, 1H, J=6 Hz), 4.60 (s, 2H), 4.45 (s, 2H), 1.40 (d, 6H, J=6 Hz); MS: 381(M+H)+.

According to the analysis of related databases, 53312-81-5, the application of this compound in the production field has become more and more popular.