Month: April 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. 38487-86-4, name is 2-Amino-4-chlorobenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C7H5ClN2

3-phenylpropiolic acid(185 mg, 1.27 mmol) was suspended in dichloromethane (1.9 ml), there to oxalyl chloride (0.114 ml, 1.33 mmol), and stirred for 2 hours at room temperature was added a DMF (1 drop). Thereto 2-amino-4-chlorobenzonitrile (194 mg, 1.27 mmol) and stirred overnight at room temperature added. After the reaction, water was added. Through a diatomaceous earth column (VARIAN Chem Elute 12198006), it was washed with chloroform. The solvent was distilled off and the residue was purified by silica gel column chromatography (SNAP 25 g, hexane / ethyl acetate) to give the title compound (268 mg, 75.2%) as a pale yellow 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.

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. 3759-28-2, name is 2-(Cyanomethyl)benzonitrile, A new synthetic method of this compound is introduced below., Product Details of 3759-28-2

General procedure: A well stirred solution of the base aromatic amine (0.01 mol) in 2 N hydrochloric acid (15 mL) was cooled in an ice-salt bath and diazotized with sodium nitrite (0.01 mol) in water (5 mL). The mixture was then tested for complete diazotization using starch iodide paper which gives a weak blue test. If the mixture does not give the test, more sodium nitrite was added dropwise until a positive test is obtained and the color is stable for few minutes. If, on the other hand, strong test for nitrite is obtained, a few drops of a dilute solution of the base hydrochloride are added until the nitrite test is nearly negative. The above cold diazonium solution was added slowly to a well stirred solution of compound 1 (1.42 g, 0.01 mol) in ethanol (20 mL) containing sodium acetate (1 g) and the mixture was cooled in an ice-salt bath. After the addition of the diazonium salt solution, the reaction was tested for coupling reaction. A drop of the reaction mixture was placed on a filter paper and the colorless ring surrounding the spot dye was treated with a drop of an alkaline solution of a reactive coupler, such as a sodium salt of 3-hydroxy-2-naphthanilide. If unreacted diazonium salt is present, a dye is formed. The presence of unreacted coupler can be determined in a similar manner using a diazonium salt solution to test the colorless ring. After the coupling reaction was complete, the reaction mixture was stirred for 15 min at room temperature to coagulate the dye particles. The precipitated deep-colored product formed was filtered off, washed with water several times, dried and crystallized from dioxane to give compounds 2a-e.

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.

185836-35-5, name is 4-(Benzyloxy)-2-fluorobenzonitrile, 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. COA of Formula: C14H10FNO

Preparation 26 tert-butyl (3R,4S)-4-(5-(benzyloxy)-2-cvanophenoxy)-3-fluoropiperidine-1-carboxylate To a solution of 4-(benzyloxy)-2-fluorobenzonitrile (WO2006016548, 1 g, 4.4 mmol) in DMF (20 ml_) was added tert-butyl-(3R,4S)-3-fluoro-4-hydroxypiperidine (JOC (2013), 78 (17), 8892-8897, 1 g, 4.84 mmol) and cesium carbonate (2.86 g, 8.802 mmol). The reaction was heated to 100C for 16 hours before cooling and diluting with EtOAc. The solution was washed with water, brine, dried over sodium sulphate and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 10% EtOAc in hexanes to afford the title compound as a yellow gum (1.7 g, 90%). 1 H NMR (400 MHz, DMSO-d6):5 ppm 1.40 (s, 9H), 1 .70-1.90 (m, 2H), 2.95-3.40 (m, 2H), 3.80-3.90 (m, 1 H), 4.00-4.15 (m, 1 H), 4.86-5.00 (m, 2H), 5.19 (s, 2H), 6.77-6.79 (m, 1 H), 6.99 (s, 1 H), 7.34-7.47 (m, 5H), 7.65-7.67 (m, 1 H). MS m/z 427 [M+H]+

The synthetic route of 185836-35-5 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 22972-63-0 as follows. category: nitriles-buliding-blocks

A solution of DIBAL ([1 M] in toluene) (1 60.9 ml_, 160.9 mmol, 2.5 eq) was added dropwise to a stirred solution of 2-(3,5-Dimethoxy-phenyl)-2-methyl-propionitrile (13.2 g, 64.36 mmol, 1 eq) in dry CH2CI2 (320 ml_) under nitrogen at -78 SC. The reaction mixture was stirred at -78 SC for 1 h. An aqueous solution of potassium sodium tartrate (10% solution in water) was added dropwise and the reaction mixture was warmed to room temperature and stirred vigorously overnight. The solid was filtered through celite and rinsed with CH2CI2, the product was extracted with CH2CI2. The combined organic layers were washed with brine and water, dried over anhydrous MgSC , filtered and the solvent was removed under reduced pressure. The product was purified by chromatography on silica gel (heptane/EtOAc, from 100:0 to 80:20). The desired fractions were collected and concentrated to afford the title product as a colorless oil. (1 1 .6 g, 86.5 %). 1 H NMR (300 MHz, CDC ) d 9.46 (s, 1 H), 6.40 (s, 3H), 3.79 (s, 6H), 1 .43 (s, 6H). LC-MS (ESI+): 209.1 (M+H+); R.T. : 1 .388 min. (HPLC Method E).

According to the analysis of related databases, 22972-63-0, the application of this compound in the production field has become more and more popular.

Reference of 326-62-5, These common heterocyclic compound, 326-62-5, name is 2-(2-Fluorophenyl)acetonitrile, 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: A mixture of nitrile (5 mmol), tert-butyl benzoate (5.5 mmol) and Zn(ClO4)2·6H2O (2 mol%) was placed in around bottom flask. Then, the reaction mixture was heated at 50 C for the given time. After completion of the reaction monitored by thin layer chromatography (TLC), the reaction mixture was quenched with 5-ml water. Then the reaction system was added 10 ml aqueous NaOH solution (1 mol/L) and continued to be stirred 5 min and extracted with ethyl acetate (3 × 10 ml). The organic layers were collected, combined, washed with water (3 × 10 ml), driedover anhydrous Na2SO4, and concentrated under vacuum.

The synthetic route of 326-62-5 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 135748-35-5, name is 4-Chloro-2,5-difluorobenzonitrile, 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 135748-35-5, HPLC of Formula: C7H2ClF2N

b 2-[[(1R)-3-Azido-1-(3-isoxazolyl)propyl]oxy]-4-chloro-5-fluorobenzonitrile The product from step (a) (0.1 g) and 2,5-difluoro-4-chloro-benzonitrile (0.18 g) and sodium hydride (60% dispersion in oil, 0.035 g) were subjected to the procedure described in Example 90(a) to afford the product as a gum (0.15 g). MS APCI+ve m/z 294 [(M-28)+].

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.

Some common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, molecular formula is C20H23FN2O2, 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. name: 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

To a 100 mL three-necked flask equipped with a stirring blade and a thermometer were added racemic 4- [4- (dimethylamino) -1- (4′-fluorophenyl) -1-hydroxybutyl] -3- (hydroxymethyl ) -benzonitrile free form (3) 10 g (29.3 mmol),45 mL of 1-butanol (4.5 parts by volume based on 1 part by mass of the free form (3)),4.4 mL of chloroform (0.44 parts by volume based on 1 part by weight of the free form (3)) was added.The resulting mixture was heated to 60 C.,30 mL of 1-butanol (3.0 parts by volume based on 1 part by mass of the free form (3)),Acetic acid in 0.4 mL of a mixed solutionA solution of 4.5 g (11.7 mmol) of (+) – di- (p-toluoyl) tartaric acid was mixed,The free form (3) was tartarylated.After tartarylation,1-butanol 75 mL (tartrate (4)9.4 parts by volume based on 1 part by mass),While maintaining the solvent composition of 4.4 mL of chloroform (0.44 parts by volume based on 1 part by weight of tartrate (4)),Seed crystal 25 mg was added,The mixture was stirred at 60 C. for 1 hour,The precipitation of crystals was visually confirmed.After precipitation of crystals was confirmed,Cooling to 20 C at a cooling rate of 20 C / hr,Further aging was carried out at the same temperature for 3 hours to precipitate crystals.After aging, crystals precipitated by vacuum filtration were filtered off,By 1 mL of 1-butanol (1 part by volume based on 1 part by mass of the free form (3)),The filtered crystals were washed twice.The obtained white crystals were dried under reduced pressure at 40 C. for 12 hours,As white crystals(10.4 mmol) of tartaric acid salt (4) (yield: 38%Chemical purity 99.83%Impurity 1 0.002%,Impurity 2 0.015%,Optical purity 98.83%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 103146-25-4, its application will become more common.

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 19924-43-7 as follows. Recommanded Product: 19924-43-7

Example 143; tert-butyl 1-isopropyl-6-((3-methoxy-6-methylpyridin-2-yl)methoxy)4-methyl-3,4-dihydroisoquinoline-2(1H)-carboxylate To a solution of methoxyphenyl acetonitrile (4.0 g, 27 mmol) in THF at room temperature was added NaH (1.19 g, 30 mmol). After 20 min, MeI (1.68 mL, 27 mmol) was added. The reaction was stirred at room temperature overnight. H2O was added to quench the reaction. It was concentrated and diluted with Ether. The ether was washed with 1N HCl, saturated NaCl, dried and concentrated to give a crude mixture which was purified by column chromatography on ISCO (120 g) with 0-30% hexanes in ethyl acetate over 28 min to yield 2-(3-methoxyphenyl)-propanenitrile (1.9 g, 44% yield) as a light brownish oil. HPLC retention time (Method C)=2.47 min. LC/MS (ESI) (M+H)+=162.16. 1H NMR (CDCl3, 400 MHz) delta ppm 1.64 (d, J=7.34 Hz, 3H), 3.82 (s, 3H), 3.85-3.92 (m, 1H), 6.83-6.96 (m, 2H), 7.24-7.34 (m, 2H).

According to the analysis of related databases, 19924-43-7, the application of this compound in the production field has become more and more popular.

76469-88-0, name is Methyl 4-(cyanomethyl)benzoate, 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. Application In Synthesis of Methyl 4-(cyanomethyl)benzoate

Step 2: 2-(4-(Methoxycarbonyl)phenyl)acetic Acid A stirred solution of methyl 4-(cyanomethyl)benzoate (22.0 g, 0.125 mol) in methanol (550 mL) was bubbled through with hydrogen chloride gas for 8 h under reflux conditions. The reaction mixture was cooled to 20 C., stirred for an additional 24 h and filtered. The filtrate was evaporated under reduced pressure. The resultant residue was dissolved in diethyl ether, washed sequentially with water and saturated aqueous sodium hydrogen carbonate, dried over sodium sulfate and evaporated to afford the methyl ester as a solid residue. 1H NMR (400 MHz, CDCl3): 8.00 (d, J=8 Hz, 2H); 7.35 (d, J=8.4 Hz, 2H); 3.91 (s 3H); 3.70 (s, 3H); 3.68 (s, 2H). GCMS: 209 (M+H). The methyl ester (8.21 g, 0.039 mmol) was dissolved in methanol, treated with sodium hydroxide (1.58 g, 0.039 mol), heated to 50 C., stirred for 4 h, cooled to room temperature, stirred for an additional 24 h and concentrated in vacuo. The resultant residue was partitioned between diethyl ether and water. The aqueous layer was acidified with concentrated HCl. The resultant precipitate was removed by filtration and dried overnight, under vacuum, to afford 2-(4-(methoxycarbonyl)phenyl)-acetic acid (80%) as an off-white solid. 1H NMR (400 MHz, DSMO-d6): 7.90 (d, J=8 Hz, 2H); 7.422 (d, J=8 Hz, 2H); 3.85 (s 3H) 3.68 (s, 2H). [M+H] 195

The synthetic route of 76469-88-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 1953-99-7, 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. 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Tetrachlorophthalonitrile (26.6 parts by weight),m-mercaptobenzoic acid (15.4 parts by weight),To a solution of dimethylformamide (200 parts by weight),Add potassium carbonate (15 parts by weight)The reaction was allowed to proceed for 1 hour at room temperature.Subsequently, thionyl chloride (50 parts by weight) was added and reacted at 70 C. for 1 hour. After cooling to room temperature, 1-methoxy-2-propanol (10 parts by weight) was added, and the mixture was further heated to reflux for 4 hours. .After completion of the reaction, liquid separation with ethyl acetate and 1N aqueous hydrochloric acid was performed.The organic layer was concentrated and purified by silica gel column chromatography. Subsequently, sodium tungstate for the purified sample(5 parts by weight), hydrogen peroxide (30%, 6.8 parts by weight) acetic acid(5 parts by weight) and ethanol (50 parts by weight) were added and stirred at 50 C. for 5 hours. After completion of the reaction, separation and purification by silica gel column chromatography gave Intermediate A-103 (10 parts by weight).

The synthetic route of 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile has been constantly updated, and we look forward to future research findings.