Month: April 2021

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.

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.

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.

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.

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 6575-13-9 as follows. SDS of cas: 6575-13-9

2,6-Dimethylbenzonitrile (10 g, 76.2 mmol),N-Bromosuccinimide (12.074 g, 68.6 mmol) and azobisisobutyronitrile (0.563 g, 3 mmol) were dissolved in anhydrous chloroform (241.42 mL), reacted at 65 C for 4 hours and extracted with dichloromethane After drying with anhydrous magnesium sulfate, purification was carried out by chromatography on silica gel (SiO2, n-Hexane: THF = 9: 1) to remove the side products to obtain a product.

According to the analysis of related databases, 6575-13-9, 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. 92616-49-4, name is 4-Bromo-1-naphthonitrile, A new synthetic method of this compound is introduced below., Formula: C11H6BrN

2-[(1H-Indol-2-yl)hydrazino]acetic acid methyl ester (2.2 g), 4-bromo-1-naphthalenecarbonitrile (2.3 g), CuI (1.0 g), Cs2CO3 (3.0 g),Dimethyl glycine (500 mg) was added to DMSO (50 mL) and replaced by argon gas. The reaction was stirred at 130 C for 12 h.After cooling to room temperature, ethyl acetate and saturated water were added to separate the layers. The ethyl acetate phase was washed twice with saturated brine, dried over anhydrous sodium sulfate and filtered.Concentration under reduced pressure and purification by column chromatography (eluent: dichloromethane:methanol = 10:1, v:v) gave 0.9 g of pure product in 24% yield.

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.

Application of 77326-36-4,Some common heterocyclic compound, 77326-36-4, name is 2-Amino-6-fluorobenzonitrile, molecular formula is C7H5FN2, 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 2;: N,N-Dimethyl-2-cyano-3-methoxyphenylsulfonamide (Compound No. 2); 2.1 : 2-Amino-6-methoxybenzonitrile; EPO A solution of 70 g (0.5 mol) of 2-amino-6-fluorobenzonitrile (prepared, e.g. according to US 4,504,660) in 250 ml of N,N-dimethylformamide was prepared, and a solution of 30.6 g (0.55 mol) of sodium methoxide in 70 ml of methanol was added dropwise at room temperature while stirring. The mixture was then refluxed for 5 hours with stirring. The completion of the reaction was monitored by TLC. An additional 25 g of sodium methoxide in 35 ml methanol were added and the reaction mixture was refluxed for an additional 4 hours while stirring. The reaction mixture was concentrated under reduced pressure. The resulting residue was triturated with water, filtered off with suction and the solids obtained were dissolved in ethyl acetate. The resulting solution was concen- trated in vacuo. The obtained residue was triturated with petroleum ether and filtered off with suction. Yield: 48 g (63% of theory) of a brownish solid having a melting point of 143-146C.

The synthetic route of 77326-36-4 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, 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: C11H19NO4

General procedure: A mixture of 0.1 mol of acetal 4 or 6-8 and 0.12 mol of 7% aqueous HCl was stirred for 3 h at 70-80C. The product was isolated by distillation.

The synthetic route of Ethyl 2-cyano-4,4-diethoxybutyrate has been constantly updated, and we look forward to future research findings.

Reference of 915394-29-5, 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. 915394-29-5, name is 2-(3-Aminophenyl)-2-methylpropanenitrile, This compound has unique chemical properties. The synthetic route is as follows.

FIG. 3C shows a modification of Scheme 1 (e.g., Scheme 1A), which uses a different Ring A reactant that results in the Ring A of the product being the structure of Compound 115. Accordingly, variations of Scheme 1 can be implemented to generate the other compounds that fall under Formula A and/or Formula B.Compound 115 is confirmed by the following spectral data: the yellow solid of Compound 115 (37.82 mg, 83.63 u mol, 34.89% yield, 95.630% purity) was confirmed by 1HNMR(EW13467-173-P1A), CNMR(EW13467-173-P1B), LCMS(EW13467-173-P1B) and HPLC(EW13467-173-P1B); LCMS: Retention time: 1.021 min, (M+H)=433.3, 5-95AB_R_220&254.1 cm. EW13467-173-P1B; HPLC: Retention time: 2.403 min, 10-80AB_4min.1 cm. EW13467-173-P1B; NMR: 1H NMR (400 MHz, DMSO-d6) ppm=9.79 (s, 1H), 8.75 (br d, J =4.0 Hz, 1H), 8.28 (br d, J =8.9 Hz, 2H), 8.09 (d, J =8.1 Hz,1H), 7.88 (s, 1H), 7.76-7.67 (m, 1H), 7.48-7.34 (m, 3H), 7.13 (br d, J =7.7 Hz, 1H), 2.69 (s, 3H), 1.72 (s, 6H).

The chemical industry reduces the impact on the environment during synthesis 2-(3-Aminophenyl)-2-methylpropanenitrile. I believe this compound will play a more active role in future production and life.

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. 4475-95-0, name is 2-Amino-2-methylbutanenitrile, A new synthetic method of this compound is introduced below., SDS of cas: 4475-95-0

5:00 g (50.94 mmol) of 2-amino-2-methylbutanonitril [synthesis described in: Lonza AG, US 5,698,704 (1997);Deng, SL et al.Synthesis 2001, 2445;Hjorringgaard, CU et al.. J. Org. Chem 2009, 74, 1329;Ogrel, A. et al.EUR. J. Org. Chem. 2000, 857] were introduced into 50 ml of THF and 6.5 ml of water, 21.83 g (157.92 mmol) of potassium carbonate and treated at 0 C slowly with 7.9 ml (56.04 mmol) Benzylchlorocarbonat (benzylchloroformate) ,After addition of 8 ml THF and 3 ml of water, the reaction mixture was stirred slowly at RT coming overnight.Then was treated with water and extracted three times with ethyl acetate.The combined organic phases were dried over sodium sulfate and concentrated.The residue was dissolved in diethyl ether and precipitated with petroleum ether.The product was filtered off, the solid washed with a little petroleum ether and dried under high vacuum.There were 11:35 g of the target compound (93%. Th.)

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.