Month: April 2021

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.

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.

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: 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, 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 74137-36-3, Product Details of 74137-36-3

The Bl (3.34g, 10 mmol) was added vial, the injection of THF dried, placed in a dry ice – acetone bath cooling, -78 ° C was added dropwise n-BuLi (1 lmmol, 2.5M) solution, stirring was continued for 3 hours and then triisopropyl borate (2.07g, 11 mmol) added to the bottle, slowly brought to room temperature and stirred overnight. After completion of the reaction, dilute HC1 solution was dropwise jerk, and extracted with methylene chloride, the organic layer was dried, solvent was removed, dichloromethane and petroleum ether (60-90) was washed with a mixture of beating to give D-1 (2.57g, y = 86percent),

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.

Adding a certain compound to certain chemical reactions, such as: 75148-49-1, name is 3-Bromobenzaldehyde Diethyl Acetal, 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 75148-49-1, Quality Control of 3-Bromobenzaldehyde Diethyl Acetal

General procedure: One equiv. of protected hydrazine was dissolved/suspended in EtOH containing 10% water (approx. 5 ml per 1 mmol of protected hydrazine), 1.05 eq of benzaldehyde acetal was added, followed by the addition of 0.05 equiv. of TsOH in an ethanolic solution (10 mg of TsOH per 0.5 ml of EtOH). The obtained reaction mixture was refluxed and monitored by TLC (silica gel) until full conversion of the starting material was observed. Ethyl acetate/light petroleum mixtures or pure ethyl acetate were used as TLC eluents. After completion of the reaction the solvent was removed under reduced pressure, approx. 15 ml of toluene was added to the residue and the solvent was again removed under reduced pressure. The obtained crude hydrazone was dissolved in commercial stabilized THF (approx. 4 ml per 1mmol of hydrazone), the flask was flushed with argon and 3 equiv. of 1M BH3-THF complex was added at room temperature, followed by 3 hours of stirring. The progress of the reaction was checked by TLC and if some unreacted hydrazone was left, stirring was continued for an additional 45 min. After thefull conversion of hydrazone EtOH (10 ml) was added to the reaction mixture (Caution: Liberation of hydrogen) and the obtained mixture was refluxed for 1 hour. After cooling to room temperature the solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate, washed with saturated NaHCO3 solution, water and saturated NaCl solution. The aqueous phase was extracted twice with ethyl acetate, the extracts were washed with saturated NaCl solution, combined with the organic phase, dried over anhydrous Na2SO4 and evaporated to dryness. The residue was purified by column chromatography on silica gel by using ethyl acetate/light petroleum 1:1 or 1:2 mixtures or pure ethyl acetate as eluent. For the exact information about the eluent used for monitoring reaction progress and chromatographic purifications, see the Rf value for each compound.

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, 3-Bromobenzaldehyde Diethyl Acetal, other downstream synthetic routes, hurry up and to see.

Reference of 538-86-3, These common heterocyclic compound, 538-86-3, name is (Methoxymethyl)benzene, 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: A sealed tube was charged with isochroman (or benzylic ether;1 mmol), DTBP (1.5 mmol), thiol (or thiophenol; 1.5 mmol). Thereaction mixture was stirred at 120 °C for 6 h. The reactionmixture was then cooled to obtain a brown liquid. The organicsolutions could be purified directly by column chromatographyon silica gel to give the pure product (hexane?EtOAc, 20:1).

The synthetic route of 538-86-3 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. 41406-00-2, name is 3-Isopropoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 41406-00-2

Example 75 Preparation of 2-fluoro-3-iodo-N-(3-isopropoxyphenyl)-4-methylbenzamideOxalyl chloride (2 M in DCM) (1832 mul, 3664 mumol) was added to a suspension of 2- fluoro-3-iodo-4-methylbenzoic acid (684 mg, 2443 mumol) in DCM (20 mL) at 0 0C. One drop of DMF (cat) was added. The mixture was stirred at RT for 3 h. Solvent was removed under vacuum. DCM (5 mL) was added to the residue and the mixture was added slowly to a mixture of 3-isopropoxybenzenamine (540 muL, 3664 mumol) and triethylamine (681 muL, 4885 mumol) in DCM (10 mL) at 0 0C. The mixture was stirred at RT overnight and then water (50 mL) was added. The mixture was extracted with DCM (3 x 50 mL). The combined organic layers were washed with brine (100 mL) and dried over sodium sulfate. The solvent was removed in vacuo and the residue was purified by preparative TLC eluting with 10% EtOAc / hexane to give the title compound (683 mg, 68%). MS (M+H)+ 414.

The synthetic route of 41406-00-2 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 7025-06-1, 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. 7025-06-1 name is 1-Bromo-2-phenoxybenzene, 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.

1-Bromo-diphenyl ether (9.8 g, 40 mmol) was added to a three-necked flask, stirred and dissolved with 200 mL of anhydrous tetrahydrofuran, protected with nitrogen, cooled to -78 C, then slowly added dropwise 2.5 M butyl lithium 16mL of solution, stir for half an hour after addingThen, a solution of 3-bromocarbazole (9.76 g, 40 mmol) in tetrahydrofuran was added dropwise to the reaction solution, and the mixture was added dropwise to room temperature, and the reaction was stirred for 2 hours.Quenched by adding a saturated ammonium chloride solution, adding a water solution, and concentrating the organic phase.A yellow oil was obtained. The oil was added to a mixture of 100 mL of HAc and 20 mL of HCl.After cooling, the organic phase was washed three times with DCM extraction of saturated brine.The solvent was evaporated and the residue was crystallised from DCM /EtOAc.The white solid was obtained as Compound 3-1 (13.4 g, yield 82%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-phenoxybenzene, and friends who are interested can also refer to it.

Related Products of 1579-40-4,Some common heterocyclic compound, 1579-40-4, name is Di-p-tolyl Ether, molecular formula is C14H14O, 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 neat mixture of p-tolyl ether (1.784 g, 9.00 mmol), 5-tertbutylisophthalic acid (1.000 g, 4.50 mmol), zinc chloride (4.478 g, 32.86 mmol) and phosphorus oxychloride (3.4 mL, 36 mmol) were heated at 100 C for 24 h under a N2 atmosphere. The mixture was cooled to room temperature to give viscous dark red-orange oil. The tacky reaction product was suspended in EtOAc (150 mL) and loosened with a spatula, before being transferred and quenched with water (250 mL) and rapidly stirred for 0.5 h. The resulting emulsion was extracted with EtOAc (3 100 mL) to give a bright orange solution. The combined organic layers were then washed with water (2 100 mL) to afford a transparent yellow solution, which was dried over Na2SO4, filtered and silica gel added. The solvent was removed by rotary evaporation and the orange silicaabsorbed crude product was purified using flash chromatography on silica gel, eluting with hexanes-EtOAc (9:1). The first colourless fraction was collected, the solvent removed under reduced pressure, yielding 1 as a white solid (1.683 g, 65%). A second slightly pink-tinged band yielded 2 as a pink tinged solid. If CH2Cl2 was used as the extracting solvent, no 2 was obtained and the yield of 1 increased to >85%. Data for 1. M.p. 199e202 C. 1 H NMR (400 MHz, (CD3)2CO): d 7.23 (d, J 1.6, 2H, phen-H), 7.21 (t, J 1.6, 1H, ArH), 7.16 (m, 4H,xan-H), 7.07 (ddd, J 8.3, 2.2, 0.5, 4H, xan-H), 7.00 (d, J 8.3, 4H, xan-H), 5.24 (s, 2H, CeOH), 2.20 (s, 12H, xan-Me), 1.13 (s, 9H, Ar-tBu). 13C{1 H} NMR (100.6 MHz, (CD3)2CO): d 150.50 (Cq), 149.64 (2 Cq), 149.01 (4Cq), 132.96 (4Cq), 130.11 (4ArCeH), 129.51 (4ArCeH), 129.26 (4Cq), 122.74 (1ArCeH), 121.81 (2ArCeH), 116.58 (4ArCeH), 70.99 (2 Cq), 35.36 (t-Bu) 31.75 (3t-Bu), 20.99 (4Ar-Me). IR (ATR): ~nmax=cm1 3746 (vw), 3667 (w), 3642 (w), 3511 (w), 2950 (w), 2916 (w), 2859 (w), 1606 (w), 1482 (s), 1436 (m), 1420 (m), 1359 (m), 1310 (m), 1284 (s), 1257 (s), 1213 (s), 1135 (s), 1110 (m), 1014 (s), 952 (m), 902 (w), 887 (m), 807 (s), 763 (m), 757 (m). ()-HR-ESI-MS: Found m/z 579.2779 (calc. [C41H38O4] : m/z 582.2770).

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

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. 1462-37-9, name is ((2-Bromoethoxy)methyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of ((2-Bromoethoxy)methyl)benzene

EXAMPLE 17; Preparation of (5S)-N {3- [3- (2-Benzyloxy-ethoxyimino)-4- methyl-3, 4-dihydro-2H-benzo [1, 4] oxazin-7-yl)-2-oxo-oxazolidin-5-ylmethyl}- acetamide; Sodium hydride (95percent, 80 mg, 3.3 mmol) is added portionwise at 0 °C to (5S)- N [3- (3-hydroxyimino-4-methyl-3, 4-dihydro-2H-benzo [1, 4] oxazin-7-yl)-2-oxo- oxazolidin-5-ylmethyl]-acetamide (from Example 9, step 1, 0.5 g, 1.49 mmol) in DMF (15 ml). The reaction mixture is stirred at 0 °C for 30 min and then benzyl-2- bromo ethyl ether (0.360 ml, 2.27 mmol) added dropwise. The reaction is allowed to warm to room temperature and stirred overnight. The reaction is quenched with sat. ammonium chloride, diluted with ethyl acetate, washed with water and brine, dried (Na2SO4) and evaporated. The residue is purified by PTLC (10percent MeOH/DCM) to give product as a white solid (0.45 g, 64percent); HPLC r. t. 5.26 min ; 1H NMR (300 MHz, CDC13-d) 8 7.28-7. 35 (m, 5H), 7.15 (d, J = 2.4 Hz, 1H), 7.09 (dd, J = 2.4, 8. 7 Hz, 1H), 6.80 (d, J = 9 Hz, 1H), 6.10 (t, 1H), 4.98 (s, 2H), 4.76 (m, 1H), 4. 58 (s, 2H), 4.13 (m, 2H), 4.02 (t, J = 9 Hz, 1H), 3.68-3. 76 (m, 4H), 3.56-3. 63 (m, 1H), 3.22 (s, 3H), 2.03 (s, 3H); MS for C24H2sN406m/z 469.0 (M+H) +.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1462-37-9.