Month: April 2021

Reference of 1535-73-5, The chemical industry reduces the impact on the environment during synthesis 1535-73-5, name is 3-Trifluoromethoxyaniline, I believe this compound will play a more active role in future production and life.

General procedure: To the stirred mixture of benzaldehyde (0.20 mL, 2.0 mmol) and amine (2.0 mmol, aniline: 0.18 mL, 4-toluidine: 0.21 g, biphenyl-4-amine: 0.34 g, 4-fluoroaniline: 0.19 mL, 4-chloroaniline: 0.26 g, 4-bromoaniline: 0.24 g, 4-nitroaniline: 0.28 g, ethyl 4-aminobenzoate: 0.33 g, 4-methoxyaniline: 0.25 g, 3,4-dimethoxyaniline: 0.31 g, 2-(methylthio)aniline: 0.25 mL, 2-aminobenzophenone: 0.39 g, 3-phenoxyaniline: 0.37 g, 3-(trifluoromethyl)aniline: 0.25 mL, 3-(trifluoromethoxy)aniline: 0.27 mL, naphthalene-1-amine: 0.29 g) was added (1.2 mL, 2.0 mmol) of T3P (Aldrich 50percent solution in EtOAc). If the mixture did not become a solution, (in the cases of the examples covered by entries 3 and 7 of Table 1) CH2Cl2 (2 mL) and EtOAc (2 mL) were added. After 5 min, (0.35 mL, 2.0 mmol) of P(OEt)3 was added and the mixture was stirred at 26 °C. After completion of the reaction (5?10 min), the mixture was diluted with EtOAc (15 mL) and washed with 10percent NaHCO3 solution (15 mL). The organic phase was dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography on silica gel (Merck 107736 Silica gel 60H, CH2Cl2?MeOH) to afford products 3a?p.

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-Trifluoromethoxyaniline, other downstream synthetic routes, hurry up and to see.

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. 19500-02-8, name is 3-Methoxy-2-methylaniline, A new synthetic method of this compound is introduced below., Safety of 3-Methoxy-2-methylaniline

The 15.0g of 3-amino-1-methoxy-2-methylbenzene mixture, 48.7g of triphosgene and 350ml of toluene was heated under reflux for 3 hours with stirring. The reaction mixture was allowed to cool and concentrated under reduced pressure to give 17.0g of 1-methoxy-3-isocyanato-2-methylbenzene.

The synthetic route of 19500-02-8 has been constantly updated, and we look forward to future research findings.

Reference of 207226-31-1, 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. 207226-31-1, name is 1,3-Dibromo-5-(trifluoromethoxy)benzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The bromide (3.0 g, 9.38 mmol), tri-nbutyl-l-elhoxyvinyl tin (3.56 g, 9.85 mmol), and PdCl2(Ph3P)2 (0.66 g, 0.94 mmol) were dissolved in toluene and the solution stirred at 95 C for 3 hours. The volatiles were removed in vac, the residue dissolved in 1,4-dioxane (20 mL), aqueous HCl (2 N, 14taunL) added, and the solution stirred rapidly at RT for 1 hour. The mixture was diluted with water (400 mL), followed by aqueous/EtOAc work-up and silica gel chromatography (EtOAc: hexanes (1:19)) to give the titled 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, 1,3-Dibromo-5-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

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.

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.

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.

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.

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.

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.

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.