Tag: M.W=200-300

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. 70591-86-5, name is 3-Bromobenzoylacetonitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H6BrNO

General procedure: To a solution of catalyst 4 (0.01mmol), 3,5-(NO2)2C6H3CO2H (0.02mmol), and alpha,beta-unsaturated aldehyde 2 (0.10mmol) in toluene (1.0mL) was added alpha-cyanoketones 1 (0.15mmol) at 0C. The resulting solution was then stirred for 48h. After complete consumption of the aldehyde (as monitored by TLC), the reaction mixture was evaporated and then loaded onto silica gel (ethyl acetate/petroleumether=1:10 to 1:7) and the products 3a-n were obtained by column chromatography. The title compound was obtained according to the general procedure (85% yield) as a mixture of two diastereoisomers (major and minor). Yellow solid; [alpha]D30=+31.3 (c 1.60, CHCl3); mp=170-172C; 1H NMR (400MHz, CDCl3): delta 7.89 (s, 1H; minor), 7.87 (s, 1H; major), 7.79 (d, J=8Hz, 1H; both diastereoisomers), 7.59 (d, J=8Hz, 1H; both diastereoisomers), 7.41-7.37 (m, 2H; both diastereoisomers), 7.33-7.28 (m, 4H; both diastereoisomers), 5.66-5.63 (m, 1H; major), 5.60-5.56 (m, 1H; minor), 3.95 (dd, J=9.6, 6.4Hz, 1H; major), 3.90 (dd, J=10.0, 6.4Hz, 1H; minor), 3.57 (d, J=4Hz, 1H; major), 3.54 (d, J=7.2Hz, 1H; minor), 2.52-2.46 (m, 1H; minor), 2.30-2.24 (m, 1H; major), 2.09-2.03 (m, 1H, both diastereoisomers); 13C NMR (100MHz, DMSO-d6): delta 162.0, 142.2, 141.9, 136.2, 133.8, 131.1, 131.0, 129.2, 128.4, 128.1, 127.7, 127.6, 121.9, 119.6, 97.4, 93.3, 88.5, 36.6, 35.9ppm; (additional peaks are observed due to diastereoisomers). IR (KBr): nu 3386.4, 2207.0, 1607.8, 1591.1, 1559.7, 1473.7, 1148.5, 1100.6, 1073.6, 950.9, 861.8, 829.0, 791.0, 765.5cm-1; d.r.: trans/cis=3.79/1; ESI-MS (m/z): 354.1 (M-H)-; HRMS(ESI): calcd for ([C18H14NO2BrNa+]): 378.0100. Found: 378.0100; enantiomeric excess: 92%, determined by HPLC (Chiralcel OD-H column, hexane/ i-PrOH 80:20, flow rate 0.7mL/min; lambda=254nm, tmajor=18.5min, tminor=11.2min).

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.

Electric Literature of 1813-33-8, These common heterocyclic compound, 1813-33-8, name is 2-Chloro-4-(trifluoromethyl)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.

General procedure: Appropriate ROH (3.00 mmol) was added topotassium tert-butoxide (3.00 mmol) solution in toluene (7 ml).1,3-Dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (DMPU, 3ml)was added to the mixture and stirred for 30 min at 80 C. Aftercooled down to ambient temperature of the reaction mixture,2-chloro-4-(trifluoromethyl)-benzonitrile (1.00 mmol) in toluenewas dropwise and stirred for 3 h at 80 C. The reaction wasquenched by adding water and extracted with EtOAc twice. Thecombined organic extracts were dried over MgSO4, filtered, andconcentrated in vacuo. The residue was purified by flash columnchromatography on silica gel using EtOAc/hexane (1:7) eluantcondition.

The synthetic route of 1813-33-8 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 1835-49-0, name is Tetrafluoroterephthalonitrile, 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 1835-49-0, SDS of cas: 1835-49-0

Reaction was conducted in the same manner as in Example 4 except that no zeolite was used. The results were that the hydrogenolysis reaction was completed in 3 hours and the hydrogen absorption was 42%. The analysis gave a conversion of 50. 4% and a reaction yield of 20. 7% (product: 2,3, 5,6-tetrafluorobenzonitrile).

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, Tetrafluoroterephthalonitrile, other downstream synthetic routes, hurry up and to see.

Some common heterocyclic compound, 1835-49-0, name is Tetrafluoroterephthalonitrile, molecular formula is C8F4N2, 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. Safety of Tetrafluoroterephthalonitrile

Dry tetrafluoroterephthalonitrile 51.02 g (98% pure, 50.0 g in terms of tetrafluoroterephthalonitrile), dry 5% Pd/C 1.0 G, Zeolite 4A powder 37. 5 g (Molecular Sieve 4A produced by Union Showa K. K. ), and toluene 200.0 g were introduced into a 500 ml stainless steel autoclave (NU-4 model produced by Nitto Koatu Co., Ltd. ), and the autoclave was purged with nitrogen. Thereafter the contents were heated to 160C under stirring, and hydrogen pressurized at a pressure higher than that in the autoclave at the above temperature by 0.1 MPa was supplied to initiate hydrogenolysis. The rate of hydrogen absorption lowered in 2 hours after the hydrogen supply was initiated, so that the pressure in the autoclave was raised by 0. 05 MPa with hydrogen.The supply of hydrogen was terminated when the hydrogen absorption was achieved at 125 mol% (based on the mol of tetrafluoroterephthalonitrile under standard conditions). The above reaction was completed in 8 hours. Cooled to room temperature, the reaction slurry was filtered, and the filtrate was analyzed with the gas chromatography analyzer. The analysis gave a conversion of 98. 0% and a reaction yield of 78. 0% (product: 2,3, 5,6-tetrafluorobenzonitrile). The solvent of the above reaction solution was removed by means of an evaporator, and the residue was distilled under reduced pressure to obtain 2,3, 5, 6-tetrafluorobenzonitrile as a fraction under 50 mmHg at 88C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1835-49-0, its application will become more common.

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. 1223434-15-8, name is Methyl 4-bromo-2-cyanobenzoate, A new synthetic method of this compound is introduced below., Formula: C9H6BrNO2

To a 50 mL round-bottorn flask was added (1 S,4S,5R)-5-[[3-(2,6-dichlorophenyl)-5-( 1-Huorocyclopropyl)-1 ,2-oxazol-4-yl]methoxy ]-2-azabicyclo[2.2.1 ]heptane 24d (120 mg,0.30 mmol, 1.0 equiv.), methyl4-bromo-2-cyanobenzoate (55 mg, 0.23 mmol, 1.0 equiv.),pota;;;sium carbonate (83 mg, 0.60 mmol, 2.0 equiv.), and DMSO (1 mL). The resultingrnix ture was stirred at ll 0C overnight After cooling to room temperature, the mixture Vas30 diluted ‘.vith of ethyl acetate and added with H20. The pH value of the solution ‘.Vas adjusted to 6 using a lM hydrogen chloride aqueous solution. The aqueous mixture was extracted withethyl acetate (1 00 mL x 2). l11e combined organic extracts were ·washed with brine (50 mL x4), dried over anhydrous sodium sulfate, and concentrated under vacuum. The residue waspurified by silica gel column chromatography eluting with ethyl acetate/petroleum ether (1 :3)5 to give methyl 2-cyano-4-[( l S,4S,5R)-5-UJ-(2,6-dichloropheny l)-5-(J -iluorocyclopropy l)L2-oxazol-4-yl]methoxy ]-2-azabicyclo[2.2.1]heptan-2-yl]benzoate 123a (90 mg, 54~~) as anoff-white solid.

The synthetic route of 1223434-15-8 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.

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.

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.

Synthetic Route of 13338-63-1,Some common heterocyclic compound, 13338-63-1, name is 3,4,5-Trimethoxyphenylacetonitrile, molecular formula is C11H13NO3, 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: the aromatic carbaldehyde (1 mole) and the appropriate substituted phenylacetonitrile (1.1 mol equiv) were added to 5% sodium methoxide in methanol and the mixture was stirred at reflux temperaturefor 2-3 h. The resulting solid was filtered off, washed with water, and finally washed with cold methanol. The obtained crude solid was recrystallized from methanol to afford the desired product as a pure crystalline solid. The characterization data for the active compounds is given in reference section.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,4,5-Trimethoxyphenylacetonitrile, its application will become more common.