Month: April 2021

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. 16588-02-6, name is 2-Chloro-5-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-Chloro-5-nitrobenzonitrile

2-Chloro-5-nitrobenzonitrile (0.91 g, 5.0 mmol) was added to the reaction flask.Ethyl piperazine-1-carboxylate (0.84 g, 5.3 mmol),Triethylamine (1.1 g, 10.9 mmol) and acetonitrile 20 mL were refluxed for 4.5 h.After the reaction, the reaction solution was cooled to room temperature, diluted with water and extracted with ethyl acetate.The organic layer was dried over anhydrous sodium sulfate, filtered and evaporated.The residue was recrystallized from ethyl acetate to give 1a, yield 71.7%

The synthetic route of 16588-02-6 has been constantly updated, and we look forward to future research findings.

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. 796600-15-2, name is 2-Chloro-4-fluoro-3-methylbenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Chloro-4-fluoro-3-methylbenzonitrile

Example 22-Chloro-4-[[(lS,2R)-2-hydroxy-2-methyl-cyclopentyl]amino]-3-methyl-benzonitrilebsoluteIn a sealed pressure vessel, a mixture of 2-chloro-4-fluoro-3-methyl-benzonitrile (1.2 g, 7.08 mmol), (lR,2S)-2-amino-l-methyl-cyclopentanol (1.63 g, 14.2 mmol) and lithium carbonate (1.10 g, 14.9 mmol) in DMSO (14.4 mL) and water (1.4 mL) is heated at 130 C overnight. After allowing the reaction to cool to room temperature, the mixture is diluted with EtOAc and washed twice with 1 N hydrochloric acid. The organic phase isconcentrated under reduced pressure and purified using radial chromatography eluting with EtOAc/hexanes (20 to 50% EtOAc/hexanes gradient). The resulting residue is repurified using radial chromatography with 1% methanol/dichloromethane. The isolated product is recrystallized with ether/hexanes, collected by filtration, and dried under reduced pressure to yield the title compound as a white solid (450 mg, 24%). A second crop (84 mg) is also isolated. LC-ES/MS m/z (35C1/37C1) 265/267 (M+l). 1H NMR (400 MHz, DMSO-d6) delta 1.16 (s, 3H), 1.71-1.73 (m, 5H), 2.12-2.13 (m, 1H), 2.14 (s, 3H), 3.46-3.50 (m, 1H), 4.93 (s, 1H), 5.26-5.30 (m, 1H), 6.63 (d, J= 8.8 Hz, 1H), 7.47 (d, J= 8.6 Hz, 1H). Chiral HPLC showed the material had an enantiomeric excess of 67%. The enantiomeric excess is determined by SFC on a CHIRALPAK AS-H (4.6 x 150 mm, 5 mupiiota) column using 20% ethanol/carbon dioxide. Flow rate: 5 mL/min. Detection: 225 nm. Isomer 1 (title compound):TR = 1.39 min; Isomer 2: TR = 1.99 min. The absolute stereochemistry of Isomer 1 (1S,2R) is known by correlation of retentions times with Isomer 1 and Isomer 2 as described inExample 3.The enantioenriched material (534 mg) is dissolved in methanol (5.5 mL) and purified in 500 mu?. injections by SFC on a CHIRALPAK AS-H (2.1 x 25 cm, 5 muiotaeta) column using 20% ethanol/carbon dioxide. Flow rate: 70 mL/min. Detection: 225 nm. The title compound is isolated as the first eluting peak, Isomer 1 (326 mg) in 99% enantiomeric excess. The enantiomeric excess is determined by SFC as described above.

The synthetic route of 796600-15-2 has been constantly updated, and we look forward to future research findings.

Related Products of 127510-96-7,Some common heterocyclic compound, 127510-96-7, name is Methyl 2-cyano-4-fluorobenzoate, molecular formula is C9H6FNO2, 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.

Example 9a) 2-Cyano-4-dimethylamino-benzoic acid methyl ester (9a)To a stirred solution of 4,03 g (22.5 mmol) 2-Cyano-4-fluoro-benzoic acid methyl ester (J. Med. Chem., 35; 24; (1992); 4613-4627) and 60.0 ml dimethylsulphoxid were added 2.23 g (27.0 mmol) dimethylamine hydrochloride and 6.54 g (47.3 mmol) potassium carbonate. The reaction mixture was stirred for 9h at 600C in an autoclave and was concentrated with high vacuum rotation evaporator at 65C. The residue was diluted with dichloromethane, washed twice with water. The combined water phases were extracted with dichloromethane. The combined dichloromethane phases were washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude was purified by column chromatography and the desired product 9a was obtained in 85% yield (3,90 g, 19.1 mmol). MS-ESI: 205 (M+ +1 , 81).Elementary analysis: C 64.69% H 5.92% N 13.72%Determined: C 64.72% H 5.95% N 13,70%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-cyano-4-fluorobenzoate, its application will become more common.

Application of 40497-11-8,Some common heterocyclic compound, 40497-11-8, name is Ethyl 2,3-dicyanopropanoate, molecular formula is C7H8N2O2, 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 ethyl 2,3-dicyanopropanoate (1.58 g, 10.38 mmol) in methanol (52 mL) and pyridine (2.52 mL, 31.14 mmol) was cooled to 10C with an ice bath. Benzenediazonium tetrafluoroborate was added in portions over 20 minutes at 10C and the reaction stirred at room temperature for 18 hours. The reaction was concentrated in vacuo and partitioned between DCM and water. The organic layer was dried over magnesium sulphate and concentrated in vacuo to afford the title compound (2.8 g, 28%). 1 H NMR (400MHz, CDCI3): delta ppm 3.62 (s, 2H), 7.05-7.25 (m, 3H), 7.36 (m, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2,3-dicyanopropanoate, its application will become more common.

These common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, 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. Application In Synthesis of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

Experiment 38. A range of experiments were conducted examining the resolution of diol with (+)- (S,S)-DTT. The general procedure is described below, and the details and results for each reaction are in table 1.Racemic diol (20 g, 58.4 mmol) was dissolved in approximately half of the solvent used for the experiment at 40 0C. (-H)-(S5S)-DTT-H2O (quantity specified in the table) was added as a solution in the other half of the solvent. The solution was held at 40 0C and was seeded within two minutes with crystals of (S)-diol. ./2(-H)-(S5S)-DTT (approximately 5 mg). Crystallisation typically began within 5-10 minutes after seeding. After 2 h at 40 0C, the temperature of the solution was lowered to 20 0C over 2 h, and the solution was held at this temperature for a further 1 h. The product was then separated by filtration, washed with the approriate solvent (2 x 20 mL) and dried overnight at 60 0C under reduced pressure.

The synthetic route of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference of 455-18-5,Some common heterocyclic compound, 455-18-5, name is 4-(Trifluoromethyl)benzonitrile, molecular formula is C8H4F3N, 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.

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.

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

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. 67832-11-5, name is 4-Bromo-2-methylbenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C8H6BrN

General procedure for coupling reaction: An oven-dried resealable Schlenk tube were charged with Pd(OAc)2 (6.7 mg, 0.03 mmol), Xantphos (34.7 mg, 0.06 mmol), 2-methylpropane-2-sulfinamide (145 mg, 1.2 mmol) and Cs2CO3 (650 mg, 2.0 mmol). The Schlenk tube was evacuated and back-filled with argon. 4-bromo-2-methylbenzonitrile (196 mg, 1.0 mmol) and dioxane (3 ml) were added and the Schlenk tube was then sealed with a Teflon screw cap and placed in a preheated oil bath at 100oC for 15 h. After cooling of the reaction mixture to room temperature, water was added and the reaction mixture was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated under vacuum. The product was purified by flash chromatography. Yield: 228 mg, 97 % [table-1, entry-5].

The synthetic route of 67832-11-5 has been constantly updated, and we look forward to future research findings.

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. 64695-82-5, name is 2-Bromo-4,5-difluorobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 64695-82-5

0362] A solution of 2-bromo-4,5-difluorobenzonitrile (218 mg, 1.00 mmol), D-leucine amide hydrochloride (185 mg, 1.10 mmol) and DIEA (0.600 mL, 3.45 mmol) in DMSO (3 mL) was stirred at 120 C for 18 h. Water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2S04, concentrated in vacuo. The residue was purified by a silica gel column, eluted with 0-50% EtOAc in hexane to give (R)-2-(5-bromo- 4-cyano-2-fluorophenylamino)-4-methylpentanamide (175 mg).

The synthetic route of 64695-82-5 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 2941-29-9, name is Cyclopentanone-2-carbonitrile, 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 2941-29-9, Computed Properties of C6H7NO

Preparation of 2-( 1 -methyl- lH-pyrazol-4-yl)-2,4,5 ,6-tetrahydrocyclopenta-[clpyrazol-3 -amine: To a solution of di-tert-butyl 1-(1 -methyl- lH-pyrazol-4-yl)hydrazine- 1,2- dicarboxylate (103 mg, 0.330 mmol) in EtOH (1.65 mL, 0.330 mmol) was added concentrated HC1 (137 mu, 1.65 mmol). The mixture was stirred at ambient temperature for 5 minutes, then cooled in an ice bath followed by addition of 2-oxocyclopentanecarbonitrile (36.0 mg, 0.330 mmol). After stirring for 5 minutes, the reaction mixture was warmed to ambient temperature overnight. The reaction mixture was concentrated and partitioned in water and DCM. After phase-separation, the aqueous layer was basified (pH 10) and then extracted with DCM (3 x 10 mL). The combined organic extracts were dried with MgS04, filtered and concentrated in vacuo. The crude material was purified by reverse-phase column chromatography, eluting with 0-100percent acetonitrile/water to afford the product as a yellow solid (4.5 mg, 6.7percent yield). MS (apci) m/z = 204.1 (M+H).

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

Electric Literature of 228421-83-8, A common heterocyclic compound, 228421-83-8, name is 3,5-Difluoro-4-(hydroxymethyl)benzonitrile, molecular formula is C8H5F2NO, 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.

To an ice cooled solution [OF 2, 6-DIFLUORO-4-HYDROXYMETHYLBENZONITRILE] (1.24 g, 7.32 mmol; see step (iii) above) and methanesulfonyl chloride (0.93 g, 8.1 mmol) in 60 mL of methylene chloride was added triethylamine (0.81 g, 8.1 mmol) with stirring. After 3 h at [0C,] the mixture was washed twice with 1M HCI and once with water, dried [(NA2SO4)] and evaporated. The product could be used without further purification. Yield: 1.61 g (89%). ‘H NMR (300 MHz, [CDCI3)] [5] 7.29 (m, 2H), 5.33 (s, 2H), 3.07 (s, 3H)

The synthetic route of 228421-83-8 has been constantly updated, and we look forward to future research findings.