Category: ethers-buliding-blocks

Synthetic Route of 1836-62-0,Some common heterocyclic compound, 1836-62-0, name is 2-(2-Methoxyphenoxy)ethylamine, molecular formula is C9H13NO2, 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: Compound 5a (100 mg, 0.42 mmol), and 2-(2-methoxyphenoxy)ethanamine (84 mg, 0.50 mmol) were added to ethanol and theresulting heterogeneous solution was reuxed for 24 h. Themixture was cooled to room temperature and ltered through a padof celite and the ltrate was concentrated under reduced pressure.The residue was puried by ash chromatography on silica-gelwith 10% methanol in ethyl acetate. Yielding 83% compound 9a(176 mg) as a white solid. Compound 9b was synthesized followingthe procedure of preparation 9a.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(2-Methoxyphenoxy)ethylamine, its application will become more common.

Reference of 349-55-3, The chemical industry reduces the impact on the environment during synthesis 349-55-3, name is 3-Methoxy-5-(trifluoromethyl)aniline, I believe this compound will play a more active role in future production and life.

3-methoxy-5- (trifluoromethyl)aniline (100 mg, 0.52 mmol) was dissolved in CHC13 (5.2 mL) and t-butyl nitrite (124 muL, 1.05 mmol) was added dropwise by syringe. Iodine (266 mg, 1.05 mmol) was added and then the reaction was slowly heated to 50C and was maintained at this temperature for an hour and thirty minutes. The reaction was then cooled to room temperature and poured into aq. NaHS03 (50 mL). The mixture was extracted with EtOAc (50 mL) and the organic extracts were washed with aq. NaHS03 (3 X 50 mL) and brine (20 mL), dried over Na2S04, filtered, and concentrated. Purification by flash chromatography with 1% to 15% EtOAc/hexanes afforded 1-iodo-3-methoxy-5-(trifluoromethyl)benzene. Rf= 0.75 (25% EtOAc/hexanes). ‘H NMR (CDC13, 500 MHz) 8 7.53 (s, 1H), 7.41 (s, 1H), 7.09 (s, 1H), 3.82 (s, 3H). Step B: 3-Methoxy-5-(trifluoromethyl)benzonitrile To a solution of 1-iodo-3-methoxy-5-(trifluoromethyl)benzene (200 mg, 0.66 mmol) in DMF (2 mL) was added CuCN (300 mg, 5.0 mmol). The reaction was stirred at 100C for 24 hours and then poured into aq. NH3 (40 mL). The mixture was extracted with EtOAc (70 mL) and the organic extracts were washed with brine (25 mL), dried over Na2S04, filtered, and concentrated. Purification by flash chromatography with 5% to 80% EtOAc/hexanes afforded 3-methoxy-5- (trifluoromethyl)benzonitrile. 0.64 (50% EtOAc/hexanes). ‘H NMR (CDC13, 600 MHz) 8 7.47 (s, 1H), 7.34 (s, 1H), 7.31 (s, 1H), 3.89 (s, 3H). Step C: 3-Methoxy-5-(trifluoromethyl)benzaldehyde A mixture of 3-methoxy-5- (trifluoromethyl)benzonitrile mg, 0.43 mmol) and Pt02 (9.8 mg, 0.043 mmol) in 88% formic acid (651 muL) was heated to 60C. The reaction was stirred at this temperature for thirty minutes. The reaction was then cooled to room temperature, diluted with hexanes (5 mL), loaded on a silica gel column, and purified with 1% to 15% EtOAc/hexanes to afford 3-methoxy-5- (trifluoromethyl) benzaldehyde. Rf= 0.56 (25% EtOAc/hexanes). ‘H NMR (CDCl3,500 MHz) 8 10.01 (s, 1H), 7.71 (s, 1H), 7.56 (s, 1H), 7.39 (s, 1H), 3.92 (s, 3H).

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-Methoxy-5-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

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. 888327-32-0, name is 4-Bromo-1-(difluoromethoxy)-2-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 4-Bromo-1-(difluoromethoxy)-2-methylbenzene

l-(4-Difluoromethoxy-3-methyl-phenyl)-cis-3,5-dimethyl-piperazine:; To 4-bromo-l- (difluoromethoxy)-2-methylbenzene (2.36 g, 10.00 mmol) in toluene (50 mL) was added cis-2,6- dimethylpiperazine (5 g, 58.14 mmol), Pd(OAc)2 (120 mg, 0.53 mmol), BINAP (380 mg, 0.61 mmol), and t-BuOK (2.2 g, 19.64 mmol). The resulting solution was stirred for 4 hours at 80C. The solution was cooled to room temperature and washed with H2O (2 X 50 mL), dried over Na2SCt, concentrated, and purified by silica gel column chromatography (10:1 CH2CWMeOH) to give 1.1 g (41%) of l-(4- (difluoromethoxy)-3-methylphenyl)-3,5-dimethylpiperazine.

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 888327-32-0.

Reference of 24878-25-9,Some common heterocyclic compound, 24878-25-9, name is 2,2′-Oxydianiline, molecular formula is C12H12N2O, 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 [Pt(MeCN)2Cl2] in hot acetonitrile (80 C) the corresponding L1 or L2 ligand was added; the reaction mixture was stirred for 72 h in the case of 2, and 24 h for 5. Then, the solution was cooled to room temperature and the solid obtained was filtered by suction.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2′-Oxydianiline, its application will become more common.

295376-21-5, name is 1-Bromo-2-fluoro-3-methoxybenzene, 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. name: 1-Bromo-2-fluoro-3-methoxybenzene

A 250ml three-necked flask was charged with 5 g (24.4 mmol) of 2-fluoro-3-methoxy-bromobenzene,13.5 g (103.74 mmol) of ethyl acetoacetate,55ml of dimethyl sulfoxide,L-proline 1.12 g (9.76 mmol),930 mg (4.88 mmol) of cuprous iodide,Under the protection of nitrogen, 32 g (97.6 mmol) of cesium carbonate was added, and the reaction was kept at 60 to 70 C for 4 to 5 hours.Stop the reaction, add 40 ml of saturated ammonium chloride solution, stir to dissolve, add 40 ml * 2 ethyl acetate for extraction, combine the ethyl acetate layers, wash the layers with saturated brine, and perform column chromatography (mobile phase ethyl acetate: petroleum ether = 1:15)5.4 g (21.3 mmol) of compound I was obtained as a pale yellow oil with a yield of 87.2%.

The synthetic route of 295376-21-5 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. 4698-11-7, name is 10-Methoxy-5H-dibenzo[b,f]azepine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 4698-11-7

Following the procedure of Example 1, but using 30% aqueous formic acid instead of the same volume of 10% aqueous sulfuric acid, the yield is 58.0 (76.6% on theoretical).

The synthetic route of 4698-11-7 has been constantly updated, and we look forward to future research findings.

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. 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6Br2O

The mixture of 1,3-dibromo-5-methoxybenzene (0.5 g,1.88 mmol), bis(pinacolato)diboron (1.05 g, 4.1 mmol), PdCl2(dppf)(140 mg, 0.23 mmol), potassium acetate (1.1 g,11.3 mmol), and DMF(40 mL) were stirred for 2.5 h at 80 C. The solvent was removed invacuo and the residue was dissolved in CH2Cl2. The solution waswashed with water and dried over magnesium sulfate. The filtratewas concentrated to dryness, and the residue was purified by flashcolumn chromatography on silica gel (eluent: petroleum ether/CH2Cl2 = 10/1), gave compound 3 as a white solid. Yield: 383 mg(56%). 1H NMR (400 MHz, CDCl3) delta (ppm): 7.87 (s, 1H), 7.42 (d,J 0.9 Hz, 2H), 3.84 (s, 3H), 1.33 (s, 24H). 13C NMR (100 MHz, CDCl3) delta (ppm): 158.56, 133.60, 122.79, 83.78, 55.33, 24.87. MS (EI): m/z 359.9.

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.

Related Products of 175278-09-8, A common heterocyclic compound, 175278-09-8, name is 4-Bromo-2-(trifluoromethoxy)aniline, molecular formula is C7H5BrF3NO, 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.

EXAMPLE 23A 4-bromo-1-chloro-2-(trifluoromethoxy)benzene A mixture of tert-butyl nitrite (1.78 mL, 15.0 mmol), copper (II) chloride (1.61 g, 12.0 mmol) and 4-bromo-2-(trifluoromethoxy)aniline (2.56 g, 10.0 mmol) in acetonitrile (40 mL) was heated to 70 C., stirred for 3 hours, cooled to room temperature, poured into 0.5M HCl, and extracted with diethyl ether. The combined extracts were washed with water and brine, dried (MgSO4), filtered, and concentrated to provide the desired product. MS (ESI(+)) m/e 275 (M+H)+.

The synthetic route of 175278-09-8 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. 1116-77-4, name is 4,4-Diethoxy-N,N-dimethyl-1-butanamine, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 4,4-Diethoxy-N,N-dimethyl-1-butanamine

Sodium nitrite (16 gm) in water (120 ml) was added slowly for a period of 30 minutes at 0 deg C to a solution of (S)-4-(4-Aminobenzyl)-2-oxazolidinone (40 gm), concentrated hydrochloric acid (46 ml) and water (480 ml) in round bottomed flask, cooled to 0 deg C and stirred for 1 hour. The above diazotized solution was added for a period of 30 minutes at 0 deg C to sodium sulfite (78.3 gm) in water (200 ml) in another round bottomed flask, cooled to 0 deg C, slowly allowed to room temperature, heated to 55 deg C and stirred for 15 minutes at 60 deg C. Added concentrated hydrochloric acid (80 ml) to the reaction mass, stirred for 16 hours at 60 deg C, nitrogen gas was applied and heated to 90 deg C. Water (80 ml) was added to the reaction mass for 15 minutes at 90 deg C, added 4-(dimethylamino)-butyraldehyde diethylacetal for a period of 40 minutes, heated to reflux, stirred for 3 hours at reflux, cooled to 25 – 30 deg C and the pH was adjusted to 7 by adding sodium hydroxide solution(30%, 230 ml). Extracted with ethyl acetate (7 X 200 ml), adjusted the pH of the aqueous layer to 10 by adding sodium hydroxide solution (30%, 100 ml), heated to 50 deg C and again extracted with ethyl acetate (8 X 200 ml) at 50 deg C. Both the organic layers were combined, dried with sodium sulfate, given carbon treatment and the solvent was distilled off completely under vacuum at 50 – 55 deg C, ethyl acetate (80 ml) was added to the reaction mass at 25 deg C, stirred for 1 hour and cooled to 10 deg C. Stirred for 30 minutes at 10 deg C, filtered the material and washed with chilled ethylacetate(20 ml) under nitrogen atmosphere and dried at 45 -50 deg C to yield 40 gm of (4S)-4-[[3-[2-(Dimethylamino)ethyl]~ 1 H-indol-5-yl]methyl]-2-oxazolidinone.(4S)-4-[[3-[2-(Dimethylamino)ethyl]-1H-indol-5-yl]methyl]-2-oxazolidinone (40 gm, Zolmitriptan) was dissolved in isopropanol (200 ml) at 25 deg C, heated to reflux, stirred for 40 minutes at reflux and slowly allowed to cool to 0 deg C. Stirred the reaction mass for 1 hour at 0 deg C, filtered the compound, washed with chilled isopropanol(40 ml) and dried at 40 – 45 deg C under vacuum to yield (4S)-4-[[3-[2-(Dimethylamino)ethyl]-1H-indol-5-yl]methyl]-2-oxazolidinone isopropanol solvate (32 gm, Zolmitriptan isopropanol solvate; HPLC purity. 99.32%). Zolmitriptan isopropanol solvate obtained above (32 gm) was dissolved in isopropyl acetate (2250 ml) at 25 deg C. Then the contents were heated to reflux and maintained for 30 minutes to form clear solution. The solution was cooled to 25 deg C during a period of 1 hour. The separated solid was filtered, washed with isopropyl acetate (160 ml) to obtain 32 gm of zolmitriptan isopropyl acetate solvate (HPLC purity: 99.8%).

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 1116-77-4.

Electric Literature of 202865-80-3, 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. 202865-80-3 name is 4-Bromo-2-fluoro-1-isopropoxybenzene, 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.

To a mixture of 2-amino-5-[3-(t-butyl)dimethyl-silanoxypropyloxy]-1-(4-methylbenzyl)benzene (54 mg, 0.14 mmol), 4-bromo-2-fluoro-1-isopropoxybenzene (32.6 mg, 0.14 mmol), dicyclohexylphosphino-2′,6′-diisopropoxy-1,1′-biphenyl (3.3 mg, 0.007 mmol), potassium t-butoxide (28.3 mg, 0.29 mmol) and toluene (2 mL) was added palladium acetate(II) (1.6 mg, 0.007 mmol) under nitrogen atmosphere, and the resulting mixture was stirred at 100 C. for 1 hour. The reaction mixture was concentrated in vacuo. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give 1-(4-chlorobenzyl)-3-[3-(t-butyl)dimethyl-silanoxypropyloxy]-6-(3-fluoro-4-isopropoxy phenylamino)benzene (69 mg, Yield: 92%) as brown oil. 1H-NMR (delta ppm TMS/DMSO-d6): 0.00 (6H, s), 0.84 (9H, s), 1.21 (6H, d, J=6.0 Hz), 1.84 (2H, q, =6.0 Hz), 2.22 (3H, s), 3.70 (2H, t, J=6.0 Hz), 3.80 (2H, s), 3.92 (2H, t, J=6.0 Hz), 4.27 (1H, q, 6.0 Hz), 6.32-6.42 (2H, m), 6.62 (1H, d, J=3.0 Hz), 6.75 (1H, dd, J=2.4 Hz, 8.4 Hz), 6.84-6.94 (1H, m), 6.97-7.08 (5H, m), 7.25 (1H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-2-fluoro-1-isopropoxybenzene, and friends who are interested can also refer to it.