Category: nitriles-buliding-blocks

Reference of 213598-11-9,Some common heterocyclic compound, 213598-11-9, name is Methyl 3-cyano-4-isopropoxybenzoate, molecular formula is C12H13NO3, 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.

4) 50L reaction kettle to add the previous step crude,2N sodium hydroxide (5 L), tetrahydrofuran (2 L) and stirred at 60 C for 1 hourTime. After cooling to room temperature, the mixture was extracted by intermittent stirring, the aqueous solution was extracted into the water phase and the ethyl acetate was taken as the organic phase. The extraction temperatureDegree of stirring, the extractant ethyl acetate and 3-cyano-4-isopropoxybenzoic acid aqueous solution contact; compared to the organic phase / aqueous phase =1, extraction temperature 37 , extraction time = 18 minutes, continuous extraction 3 times, the separation of the aqueous phase, the organic phase was distilled off under reduced pressure, analysisA large amount of white solid was obtained to give 1.1 kg of white solid. The yield was 84% in two steps and 98.5% by HPLC.

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

Application of 16532-79-9, These common heterocyclic compound, 16532-79-9, name is 4-Bromophenylacetonitrile, 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: Toa solution of 2-bromobenzyl cyanide (20.0 g, 0.1 mol) in THF (100 mL) was added1M BH3·THF (200 mL, 0.2 mol) dropwise at 0 oCover 30 min and then heated to reflux for 24 h. After quenchedwith MeOH (50 mL) and 6M HCl (50 mL) at 0 oC, the reaction mixturewas heated to reflux for another 4 h and concentrated under reduced pressure.The residue was diluted with H2O (300 mL) and washed with EA (75 mL×2). The aqueous layer was then neutralized by 15% NaOH, extracted with EA (75mL ×2). The combined organic layer was dried over Na2SO4and concentrated under reduced pressure to afford compound 2a as yellow oil (17.4 g, 85.2%).

The synthetic route of 16532-79-9 has been constantly updated, and we look forward to future research findings.

Application of 4426-11-3, 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. 4426-11-3, name is Cyclobutanecarbonitrile, This compound has unique chemical properties. The synthetic route is as follows.

(a) A solution of borane-tetrahydrofuran complex [(1M] in tetrahydrofuran, [120ML)] was added over [10MIN] to a solution of cyclobutane carbonitrile (8. [1G)] [Lancaster] in dry tetrahydrofuran [(20ML)] under nitrogen at room temperature. The solution was refluxed overnight then cooled to [20.] Methanol [(150ML)] was added dropwise over 15mins keeping the temperature below [25,] then the mixture was cooled to [0 AND] dry hydrogen chloride was bubbled through for 30min. The resulting mixture was refluxed for 90min, evaporated and the residue re-evaporated twice from methanol. Ether [(150ML)] was added and the resulting solid was filtered off. It was taken up in hot isopropanol [(50ML),] filtered, and hot acetonitrile [(30ML)] added. The mixture was cooled and the solid filtered off to give the [C-CYCLOBUTYLMETHYLAMINE] hydrochloride (5.7g) NMR (400 MHz, DMSO-d6) F6382 1.8 (4H, m), 2.0 (2H, m), 2.54 [(1H,] m), 2.80 (2H, d), 8.0 (3H, [BR S).]

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

Some common heterocyclic compound, 144797-57-9, name is 4-Chloro-3,5-difluorobenzonitrile, molecular formula is C7H2ClF2N, 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. Recommanded Product: 144797-57-9

A solutionof 4-chloro-3,5-trifluorobenzonitrile (2) (5.0 g, 28.9 mmol) inconcentrated H2SO4 (98%, 92.0 g) was stirred for 1 h in an ice-bath.After being treated dropwise with the mixture of concentrated HNO3(65%, 2.0 g) and H2SO4 (98%, 2.2 g), the ice-bath was removed andthe mixture was stirred for another 6 h at about 102 . The reactionprogress was monitored by TLC (30% ethyl acetate in hexane). Aftercomplete conversion of compound 2, the reaction mixture was cooledto 0 by ice-bath, then treated dropwise with sodium nitrite solution(4.0 g in 25 mL water). After the addition, the mixture was stirred foranother 20 h at 120. The reaction progress was monitored by TLC(30% ethyl acetate in hexane). After cooling to room temperature,the reaction mixture was extracted with ethyl acetate (2×20 mL) andthe combined organic phases were dried over Na2SO4. The solventwas removed under reduced pressure to afford a white solid (6.9 g).The crude product was purified by using 20% ethylacetate:hexaneas eluent through column chromatography. The solvent was removedunder reduced pressure to afford a yellow solid 3 (6.5 g) in 94.9%yield.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 144797-57-9, its application will become more common.

These common heterocyclic compound, 65610-13-1, name is 3-Fluorophthalonitrile, 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. COA of Formula: C8H3FN2

A mixture of 3-fiuoro-l,2-cyanobenzene (2.49g), glycine ethyl ester hydrochloride(2.49g) and potassium carbonate (5.18g) in acetonitrile (25mL) was heated to reflux for24 hours. After cooling, the reaction mixture was extracted into dichloromethane, washedwith water, dried (MgSCU) and the solvent removed hi vacuo to yield crude productwhich was purified using flash chromatography to yield (2,3-dicyano-phenylamino)-acetic acid ethyl ester (840mg).A mixture of (2,3-dicyano-phenylamino)-acetic acid ethyl ester (453mg), triethylamine(0.24mL), di-tert-butyl dicarbonate (447mg) and 4-ditnethylaminopyridine (20mg) wasstirred in dichloromethane (5mL) at room temperature overnight. The reaction mixturewas then extracted into dichloromethane, washed with water, dried (MgSO4) and thesolvent removed in vacuo to yield crude product which was purified using flashchromatography to yield the title compound (606mg).

The synthetic route of 3-Fluorophthalonitrile 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 42872-74-2 as follows. Safety of 3-Bromo-4-methylbenzonitrile

A solution of 3-bromo-4-methylbenzonitrile (1.0 g) in EtOH (20 mL) was saturated at 0 C. with gaseous HCl and the solution was stirred at rt for 2 h. The volatiles were removed under reduced pressure and the residue was dissolve in EtOH (9 mL). Formohydrazide (0.45 g) and triethylamine (2.8 mL) were added and the solution was stirred at 90 C. for 2 h. Water (50 mL) was added and the mixture was extracted with EtOAc. The combined organic layers were dried and the volatiles were removed under reduced pressure. The residue was purified by column chromatography (Interchim cartridge 30SiHP, 40 g, Cy/EtOAc) to yield the desired product (40% yield). LC-MS (Method 1): m/z [M+H]+=238.1 (MW calc.=238.08); Rt=3.3 min.

According to the analysis of related databases, 42872-74-2, the application of this compound in the production field has become more and more popular.

Synthetic Route of 7357-70-2,Some common heterocyclic compound, 7357-70-2, name is 2-Cyanothioacetamide, molecular formula is C3H4N2S, 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 stirred solution of 2-cyanothioacetamide (3.52 g, 35 mmol) and ethyl 2,4- dioxovalerate (5.0 g, 32 mmol) in anhydrous EtOH (75 mL) at room temperature was added triethylamine (0.5 mL) and the reaction was stirred overnight. Filtration and washing of the precipitates with EtOH gave [3-CYANO-2-MERCAPTO-6-METHYL-ISONICOTINIC] acid ethyl ester as a yellow solid (4.54 g, 64.5%). A mixture of this ester (3.54 g, 16 mmol), bromoacetamide (2.15 g, 16 mmol) and sodium ethoxide (2.18 g, 32 mmol) in MeOH was heated at reflux overnight. It was then allowed to cool to room temperature. Filtration and washing of the precipitates with EtOH provided 3-amino-2-carbamoyl-6- methyl-thieno [2, [3-B]] pyridine-4-carboxylic acid ethyl ester as a solid (0.94 g, 21. [1%).]

The synthetic route of 7357-70-2 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 5922-60-1, name is 2-Amino-5-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 5922-60-1, Formula: C7H5ClN2

Preparation 237N-(4-Chloro-2-cyanophenyl)-N-(methylsulfonyl)methanesulfonamide10726] To a solution of 2-amino-5-chloro-benzonitrile (5.00 g, 32.77 mmol) in pyridine (100 mE) at 0°C. was added methanesulphonylchloride (10.21 mE, 131.07 mmol) andthe reaction stirred at room temperature for 18 hours. The reaction was concentrated in vacuo and partitioned between 2N HC1 and EtOAc. The organic layer was collected, washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was triturated with 1:1 acetonitrile:ether to afford the title compound (8.00 g, 79percent).10727] ?H NMR (400 MHz, DMSO-d5): oe ppm 3.61 (s, 6H), 7.90 (d, 1H), 7.98 (dd, 1H), 8.31 (d, 1H).

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.

Related Products of 3047-38-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3047-38-9 name is Cyclopent-1-enecarbonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Step 1: 3-bromocyclopent-1-enecarbonitrile To a stirred solution of cyclopent-1-enecarbonitrile (50 g, 537 mmol) in tetrachloromethane (400 ml) at 25 C. was added was added N-bromosuccinimide (96 g, 537 mmol) under nitrogen atmosphere. The resulting mixture was refluxed for 2 h. The progress of reaction was monitored by TLC. The reaction mixture cooled to 25 C. and filtered through celite. The filtrate was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 1% ethyl acetate in hexane as an eluent to obtain the title compound (60 g, 65%). 1HNMR (CDCl3, 400 MHz): delta 6.77-6.73 (m, H), 5.12-5.09 (m, 1H) 2.95-2.86 (m, 1H) 2.67-2.42 (m, 3H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Cyclopent-1-enecarbonitrile, and friends who are interested can also refer to it.

Synthetic Route of 916792-13-7, These common heterocyclic compound, 916792-13-7, name is 4-Bromo-2-fluoro-5-methylbenzonitrile, 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: The requisite aryl boronate derivative was prepared from the corresponding aryl bromide via reaction with 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-l,3,2-dioxaborolane in the presence of [1,1′- bis(diphenylphosphino)ferrocene]dichloropalladium(l l) and potassium acetate.

The synthetic route of 916792-13-7 has been constantly updated, and we look forward to future research findings.