Month: April 2021

Synthetic Route of 939-83-3, A common heterocyclic compound, 939-83-3, name is 2-Methyl-5-nitrobenzonitrile, molecular formula is C8H6N2O2, 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.

A mixture of 2-cyano-4-nitrotoluene (10 g, 6.17 mmol) benzaldehyde (6.51 g, 6.17 mmol) and potassium carbonate (20 g) in MeOH (200 mL) was heated at reflux for 10 min. The mixture was cooled to ambient temperature over 30 min, whereupon precipitation of the product was complete. The product was isolated by filtration and washed successively with 1N HCl, water and MeOH then air dried. There was obtained 13.0 g of the benzamide (mp 269.8 C) as evident from the lack of a nitrile adsorption in the IR and the appearance of peaks at 3357.1, 3193.6 (-NH2) and 1648.7 cm-1 (H2NC(=O)-); LRMS (M-NO)+ m/z = 238.

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 34916-10-4, These common heterocyclic compound, 34916-10-4, name is 4-Oxo-cyclohexanecarbonitrile, 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.

A solution of (Diethylamino)sulfur trifluoride (46.7 g, 289 mmol) in DCM (200 mL) was slowly added to a solution of 4-oxocyclohexanecarbonitrile (32.4 g, 263 mmol) in DCM (400 mL) at 0C. The reaction mixture was stirred for 2 hrs. and quenched with water (100 mL). The organic layer was separated and dried with anhydrous MgSO4. The solvent was concentrated to provide a 7:3 mixture of 4,4-Difluorocyclohexanecarbonitrile and 4-fluorocyclohex-3-ene-l-carbonitrile. MCPBA 77% (45 g, 200 mmol) was stirred in CHCl3 (600 mL) for 30 min. The solution was dried with anhydrous Na2SO4 and filtred. The 7:3 mixture of 4,4-Difluorocyclohexanecarbonitrile and 4-fluorocyclohex-3-ene-l- carbonitrile was added to the resulting MCPBA solution and stirred at ambient temperature for 18 hrs. The reaction mixture was washed with NaOH 1.5 M (3 x 300 mL) and dried with anhydrous MgSO4. The solvent was concentrated and the residue was distilled under reduced pressure to provide the pure title compound as a colorless liquid. Yield 18.2 g (47%): IHNMR (400 MHz, CHLOROFORM) delta 1.86-1.96 (m, 1 H), 1.95-2.03 (m, 5 H), 2.03-2.22 (m, 2 H), 2.68-2.85 (m, 1 H). EPO [(4,4-Difluorocyclohexyl)methyI]amine

The synthetic route of 34916-10-4 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 151-18-8 as follows. Recommanded Product: 151-18-8

5 L of an aqueous solution containing 500 g of beta-aminopropionitrile (previously adjusted to pH 8.0 with concentrated hydrochloric acid) was added to a 10-L jacketed mechanically stirred glass reactor.Further, 250 g of a Nitrile hydrolyzing enzyme resting cell prepared by the method described in the patent CN 101701222B was added thereto, and fully suspended by mechanical stirring (250 rpm), and the temperature of the reaction vessel was controlled to 35 C by a constant temperature water bath, and the reaction time was 6 hours.The progress of the reaction was monitored by HPLC during this time.After the substrate was completely transformed, the reaction solution was heated to 90 C, incubated for 30 min, and the cells and denatured proteins were removed by filtration.The filtrate was concentrated and dried to give a mixture of beta-alanine and buffer salt as a solid, which contained 625 g of beta-aminopropionic acid in a yield of 98.4%.

According to the analysis of related databases, 151-18-8, the application of this compound in the production field has become more and more popular.

Related Products of 1129-35-7, 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. 1129-35-7, name is Methyl 4-cyanobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Hydrazine hydrate 64% (v/v) (30.0 mL, 0.33 mol) was heated up to 50-60 C. The methyl ester 3 (0.01 mol) was added and the mixture was heated at reflux for 10 min. The cooling was performed sequentially in water bath, followed by ice bath and dry ice-ethanol bath. The precipitate was filtered and washed with cold water.

The chemical industry reduces the impact on the environment during synthesis Methyl 4-cyanobenzoate. I believe this compound will play a more active role in future production and life.

Synthetic Route of 70484-01-4, 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. 70484-01-4, name is 4-Bromophthalonitrile 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, H001-3 (15 mmol), cuprous iodide (30 mmol),t-BuOK (20 mmol) and 3,4-dicyanobromobenzene (30 mmol) were mixed with dry 1,4-dioxane (100 ml) and stirred at room temperature for 48 hours under a nitrogen atmosphere.The resulting intermediate was added to water, then filtered through a pad of celite, and the filtrate was extracted with dichloromethane.It was then washed with water and dried over anhydrous magnesium sulfate. After filtration and evaporation, the crude product was purified by silica gel column chromatography to obtain the intermediate product H002.

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

Electric Literature of 327056-73-5, The chemical industry reduces the impact on the environment during synthesis 327056-73-5, name is 3-Chloro-5-fluorobenzonitrile, I believe this compound will play a more active role in future production and life.

EXAMPLE 2 ^_(4-{(lJR)-14(R)-(3-CHLORO-5-CYANOPHENOXY)(4- CHLOROPHENYL)METHYL]BUTYL}BENZOYL)~beta-ALANINETo a solution of INTERMEDIATE 1 (100 mg, 0.239 mmol) and 3-chloro-5- fluorobenzonitrile (40.9 mg, 0.263 mmol) in DMF (2 mL) was added potassium tert-butoxide (107 nig, 0.957 mmol), then the resulting mixture was allowed to stir at 120 0C for 16 hours. After being allowed to cool to RT, the mixture was diluted with 2 N HCl (aq) then extracted with EtOAc. The organic layer was washed twice with water then concentrated. The resulting yellow residue was purified by preparative reverse phase HPLC eluting with 30-100% CHaCN/water + 0.1% TFA. Following lyophilization, this afforded the title compound as a white solid. 1H NMR (500 MHz, CD3OD): 6 7.70 (d, J – 8.5 Hz, 2 H); 7.34 (d, J = 8.5 Hz, 2 H); 7.30 (d, J = 8.0 Hz, 2 H); 7.25 (d, J – 8.5 Hz, 2 H); 7.20 (s, 1 H); 7.09 (s, 1 H); 7.06 (s, 1 H); 5.55 (d, J = 6.5 Hz, 1 H); 3.61 (t, J = 7.0 Hz, 2 H); 3.16 (m, 1 H); 2.62 (t, J = 7.0 Hz, 2 H); 1.80 (m, 1 H); 1.54 (m, 1 H); 1.11-1.07 (m, 2 H); 0.78 (t, J = 7.2 Hz, 3 H); LC3 3.93 min. (M+H)+ 523.

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-Chloro-5-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Electric Literature of 6136-93-2, These common heterocyclic compound, 6136-93-2, name is 2,2-Diethoxyacetonitrile, 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.

Sodium methylate (54 g, 1 mol) was added to a solution of diethoxyacetonitrile (139 mL, 1 mol) in methanol (500 mL). The reaction mixture was kept at room temperature for 24 g, then the reaction mixture was evaporated, treated with water (500 mL), and the product was extracted with ether (2×300 mL). The combined organic extracts were dried over anhydrous K2CO3 and evaporated to give 114.62 g (60% purity) of methyl 2,2- diethoxyethanimidoate. The obtained crude product was used for the next stage without additional purification.

The synthetic route of 6136-93-2 has been constantly updated, and we look forward to future research findings.

Related Products of 19179-31-8,Some common heterocyclic compound, 19179-31-8, name is 3,5-Dimethoxybenzonitrile, molecular formula is C9H9NO2, 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.

An oven-dried three-necked flask was sealed with septa and evacuated/backfilled with N2 several times before starting the reaction. To a mixture of 2.5 M n-BuLi in hexane (4.2 mL, 10.45 mmol) and dry THF, maintained at below -70 C, a solution of N,N-diethyl-2-methylbenzamide (1 g, 5.23 mmol) and 3,5-dimethoxybenzonitrile (1.11 g, 6.79 mmol) in dry THF was added dropwise, maintaining the temperature below -60 C. The reaction mixture was stirred at -78 C. The reaction mixture was warmed to room temperature and quenched with water. The resulting mixture was extracted with CH2Cl2, the organic extract washed with water, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was then purified by column chromatography (n-hexane:EtOAc = 1:1) to obtain compound 5b as white crystals (1.1 g, 74%). Melting point (mp): 170-173 C. 1H NMR (400 MHz, DMSO-d6): delta 11.56 (s, 1H, NH), 8.21-8.19 (m, 1H, 8-H), 7.75-7.70 (m, 2H, Ar-H), 7.52-7.46 (m, 1H, Ar-H), 7.00 (s, 1H, 4-H), 6.97 (d, J = 2 Hz, 2H, 2,6-(H)2), 6.57 (t, J = 2.2 Hz, 1H, 4-H), 3.83 (s, 6H, 3,5-(OCH3)2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Dimethoxybenzonitrile, its application will become more common.

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. 859855-53-1, name is 3-Amino-4-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H5FN2

1.0 g (6.4 mmol) of 2-fluoro-5-cyanoaniline was dissolved in anhydrous dichloromethane in a 25 ml eggplant flask,Dropping at room temperature2.3 g (9.6 mmol)2-chloro-3-methoxybenzenesulfonyl chloride in dichloromethane,Further 0.77 ml (9.6 mmol) of pyridine,Room temperature reaction overnight.The reaction solution was spin-dried to give 0.97 g (yield 48.5%) of intermediate E as a pale yellow solid

According to the analysis of related databases, 859855-53-1, the application of this compound in the production field has become more and more popular.

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 179898-34-1 as follows. COA of Formula: C7H3BrFN

Example 15 1,1-Dimethylethyl [(3-bromo-5-fluorophenyl)methyl]carbamate NaBH4 (1.99 g, 52.5 mmol) was cautiously added to a solution of NiCl2 (1.36 g, 10.5 mmol), Boc2O (4.58 g, 21.0 mmol) and 3-bromo-5-fluorobenzonitrile (2.10 g, 10.5 mmol) in absolute ethanol (30 mL) at 0 C. (vigorous reaction with the formation of a black precipitate). Once the reaction had subsided the mixture was left to stir at room temperature for 30 min. Ethanol was removed under reduced pressure and the precipitate was dissolved in EtOAc, filtered and repeatedly washed with EtOAc. The combined organic phases were washed with saturated NaHCO3, and dried (Na2SO4). After removing the solvent, the product, was purified by flash column chomatography to yield 1,1-dimethylethyl [(3-bromo-5-fluorophenyl)methyl]carbamate (2.20 g, 69%). 1H NMR (400 MHz, CDCl3) delta 1.46 (S, 9H), 4.28-4.32 (m, 2H), 4.87 (br, 1H), 6.93-7.29 (m, 3H); 13C NMR (100 MHz, CDCl3) delta 20.3, 43.6, 44.1, 79.7, 80.0, 113.0, 114.0, 117.7, 122.5, 126.0, 123.0, 141.7, 155.9, 161.5, 164.0.

According to the analysis of related databases, 179898-34-1, the application of this compound in the production field has become more and more popular.