Category: ethers-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 91-16-7, name is 1,2-Dimethoxybenzene, belongs to ethers-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 91-16-7, category: ethers-buliding-blocks

A solution of 1,2-dimethoxybenzene (10 g, 72.4 mmol) in dichloromethane(50 ml) was added dropwise to a suspension of anhydrous FeCl3 (35.22 g, 217.2 mmol) in dichloromethane (100 ml) and concentrated sulphuric acid (0.5 ml). After complete addition (15 min), the reaction mixture was further stirred for 3 h at room temperature. 200 ml of methanol were then slowly added under vigorous stirring. The obtained mixture was further stirred for additional 30 min. And the precipitate was filtered off, washed with methanol (5 × 100 ml) and dried under reduced pressure to give a purple solid. Yield: 80%, 1HNMR (CDCl3) delta/ppm: 4.10 (s, 18H, OCH3), 7.80 (s, 6H, ArH).

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, 1,2-Dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 450-91-9, name is 4-Fluoro-2-methoxyaniline, belongs to ethers-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 450-91-9, Recommanded Product: 450-91-9

4-Fluoro-2-methoxyaniline (2.4 g, 17.00 mmol)Was added portionwise to concentrated H2SO4 (15 mL) cooled in an ice / water bath,The temperature was maintained below 15 & lt; 0 & gt; C during the addition.The mixture was stirred until all of the formed solids had dissolved.KNO3 (0.815 mL, 17.00 mmol) was added in portions,So as to keep the temperature below 10 C. The mixture was stirred overnight and then poured onto ice / water.The mixture was basified with concentrated NH4OH. The resulting solid was filtered off,Then dissolved in CH2Cl2, washed with water, dried (Na2SO4),Concentrated on silica gel. Using FCC for purification,Eluting with 50% by weight of heptane in CH2Cl2,The title compound was obtained as a yellow crystalline solid (2.450 g, 77%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Fluoro-2-methoxyaniline, and friends who are interested can also refer to it.

Synthetic Route of 38197-43-2, A common heterocyclic compound, 38197-43-2, name is 2-Bromo-1-methoxy-3-methylbenzene, molecular formula is C8H9BrO, 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.

Step A: 2-methoxy-6-methylbenzonitrile: To a flask containing a stir bar was added 2-bromo-l- methoxy-3-methylbenzene (7.5 g, 37 mmol), CuCN (6.7 g, 75 mmol) followed by addition of DMF (60 mL); the resulting mixture was then refluxed at 150 C overnight. When the reaction was complete, as evidenced by LC analysis, the reaction flask was taken out of the oil bath and cooled to room temperature. To the reaction mixture was then poured DCM (20 mL) and a precipitate formed immediately. The solids were filtered, re-dissolved in DCM, absorbed into silica gel and and loaded into column with Hexanes:EtOAc (1 : 1) to afford the title product.

The synthetic route of 38197-43-2 has been constantly updated, and we look forward to future research findings.

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. 59557-91-4, name is 4-Bromo-2-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Bromo-2-methoxyaniline

At room temperature, concentrated sulfuric acid (185 mL) and deionized water (144 mL) were added with mechanical stirring in a three-necked flask.Glycerol (768.5 mmol, 207.5 g) was added and the temperature was lowered to room temperature. Sodium 3-nitrobenzenesulfonate (733 mmol, 165 g) was added in portions and the reaction was carried out at 80 C for 3 hours, 4-bromo-2-methoxyaniline (compound shown by the formula (I-1)) (495 mmol, 100.0 g) was added portionwise with vigorous stirring to giveHeat to 120 C and react overnight. Add water (600 mL) and adjust pH to approx. 7.0 with concentrated aqueous ammonia. Extract with water and ethyl acetateAfter the extraction, the organic phase was dried over anhydrous sodium sulfate, filtered, and the solvent was spinned to give 103 g of tan by column chromatographyThe oily product (compound represented by the formula (I)) had a yield of 87.4% and a purity of 94%.

The synthetic route of 59557-91-4 has been constantly updated, and we look forward to future research findings.

2132-62-9, name is 1,2-Bis(4-methoxyphenyl)ethyne, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C16H14O2

take 1,2-dicarbonylmethyl ester-Indolizine 46.6mg (corresponding to 0.20 mmol), 71.5 mg (equivalent to 0.30 mmol) of 1,2-bis(4-methoxyphenyl) acetylene, 4.5 mg of palladium acetate (equivalent to 0.02 mmol), Potassium acetate was 5.0 mg (equivalent to 0.01 mmol), 1.5 ml of dimethylsulfoxide and then stirred under heating at 130 C for 1 hours under 1 atmosphere of oxygen and separated to obtain the sixth number target Product 78.9 mg (yield 84%).

The synthetic route of 2132-62-9 has been constantly updated, and we look forward to future research findings.

Application of 16452-01-0, A common heterocyclic compound, 16452-01-0, name is 3-Methoxy-4-methylaniline, molecular formula is C8H11NO, 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: In a threaded ACE glass pressure tube with a sealed Teflon screw cap equipped with a magnetic stirring bar, a mixture of 11a (0.200 g, 1.65 mmol), 12a (0.185 g, 1.65 mmol), p-TsOH (0.028 g, 0.16 mmol), and MS 4A (0.20 g) in toluene (10 mL) was stirred and heated at 130 C for 4.5 h under microwave irradiation (100 W). The solvent was removed under vacuum and the residue purified by column chromatography (silica gel, hexane-EtOAc, 98:2) to give 7a (0.32 g, 91%) as a brownish oil; Rf = 0.75 (hexane-EtOAc, 7:3).

The synthetic route of 16452-01-0 has been constantly updated, and we look forward to future research findings.

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. 116557-46-1, name is 3-Bromo-2-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Bromo-2-methoxyaniline

[00238j To a reaction vial charged with 3-bromo-2-methoxyaniline (1.12 g, 5.54mmol), 1 -methyl-4-(4,4,5 ,5 -tetramethyl- 1,3 ,2-dioxaborolan-2-yl)- 1 H-pyrazole (1.499 g,7.21 mmol) in dioxane (6 mL) was added aqueous potassium phosphate (2.0 M) (5.54 ml,11.09 mmol). The resulting mixture was deoxygenated by bubbling argon through themixture for 5 minutes. [1,1 ?-Bis(diphenylphosphino)ferrocene] dichloropalladium(II)(PdC12(dppf), 0.122 g, 0.166 mmol) was then added and the mixture was heated at 110 Cfor 2 hours. The reaction was cooled, diluted with ethyl acetate (200 mL), washed with water, brine, dried over anhydrous sodium sulfate, filtered and concentrated to afford tan oil as the crude product mixture. This material was purified by silica gel flash chromatography using hexanes/ethyl acetate mixtures as the eluent. Fractions containingthe desired product were collected, combined, and concentrated under vacuum to afford0.87 g (77%) of the desired product as an oil which solidified upon standing. HPLC (Method N) = 0.89 minutes. LCMS MH+ 204.1.

According to the analysis of related databases, 116557-46-1, the application of this compound in the production field has become more and more popular.

Electric Literature of 578-57-4, These common heterocyclic compound, 578-57-4, name is 1-Bromo-2-methoxybenzene, 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: To a solution of brominated aromatic compounds (1 equiv),bis(pinacolate)diboron (1.5 equiv) and anhydrous ethanol (15 mL)were added10%palladium-carbon (0.01 equiv), followed by potassium acetate (3 equiv) under argon. The mixture was heated in a 60 C with stirring for the indicated time. Thereactor was cooled to room temperature, and the reaction mixture was filtered, and thefiltrate was concentrated under reduced pressure. The residue was extracted with dichloromethane (20 mL×3), and organic layer was washed with water (20 mL×2)and once with brine (25 mL), dried over magnesium sulfate and concentrated in vacuo.The product was purified by silica gel flash chromatography on silica gel usingpetroleum as eluent.

The synthetic route of 578-57-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 20781-20-8, These common heterocyclic compound, 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, 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 a solution of compound 58 (6.6 g, 33.5 mmol) in dichloromethane (100 mL)were added DIPEA (8.65 g, 67 mmol), HOBt (5.4 g, 36.85 mmol) and EDCI (9.6 g, 50.3mmol). After about 15 mm stirring, to the homogeneous reaction mixture was added asolution of 2,4-dimethoxybenzyl amine (5.6 g, 33.5 mmol) in dichloromethane (50 mL)dropwise under nitrogen atmosphere. The resulting mixture was stirred under nitrogenatmosphere at room temperature for 16h. The reaction mixture was washed successively with iN NaOH (100 mL), water (100 mL) and brine (100 mL). The organic phase was then dried over Na2SO4 and evaporated to give a crude solid product 59 that crystallized from ethyl ether. Filtration and open air suction drying afforded an off-white solid pureproduct 9.8g (96%), (MS: [M+1] = 347).

Statistics shows that (2,4-Dimethoxyphenyl)methanamine is playing an increasingly important role. we look forward to future research findings about 20781-20-8.

Reference of 36805-97-7,Some common heterocyclic compound, 36805-97-7, name is 1,1-Di-tert-butoxy-N,N-dimethylmethanamine, molecular formula is C11H25NO2, 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.

2,6-Dichloro-isonicotinic acid (11.2 g, 57.1 mmol) is suspended in toluene (150 mL) at 800C and then treated with N,N-dimethylformamide di-tert.-butyl acetal (50 mL, 209 mmol).The dark mixture is stirred at 800C for 12 h, then at rt for 16 h. The dark solution is diluted with diethyl ether (400 mL), washed with sat. aq. NaHCO3 solution (3×100 mL), dried overNa2SO4, filtered and concentrated. The crude product is purified by MPLC on silica gel eluting with heptane:ethyl acetate to give 2,6-dichloro-isonicotinic acid tert. -butyl ester (14.2 g) as a brownish oil which slowly solidifies; LC-MS: tR = 1.05 min; 1H NMR (D6-DMSO): £1.56 (s, 9 H), 7.85 (s, 2 H).

The synthetic route of 36805-97-7 has been constantly updated, and we look forward to future research findings.