Tag: M.W=200-300

Application of 175278-17-8, A common heterocyclic compound, 175278-17-8, name is 2-Bromo-4-(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.

General procedure: Triphosgene (0.14 g, 0.48 mmol) was dissolved in anhydrous CH2Cl2 (15 mL) and the mixture was stirred on the ice-bath for 15 min. 3-Bromo-5-(trifluoromethyl)aniline (0.3 g, 1.2 mmol) in anhydrous CH2Cl2 (10 mL) was added dropwise to the above mixture and stirring continued for 20 min. Et3N (0.2 mL, 1.44 mmol) diluted with CH2Cl2 (5 mL) was then added into the mixture. Stirring was continued for 20 min and a solution of Et3N (0.2 mL, 1.44 mmol), 4-pyridin-3-ylaniline (5) (0.2 g, 1.2 mmol) in anhydrous CH2Cl2 (20 mL) was added. After completion of the action, the reaction was quenched with dilute Na2CO3. The organic layer was washed with water and brine, and dried over Na2SO4. After filtration and concentration in vacuo, the residues was purified by silica gel flash chromatography (PE/AcOEt = 6:1) yielding (L1). yield 73%

The synthetic route of 175278-17-8 has been constantly updated, and we look forward to future research findings.

Reference of 29578-83-4, 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. 29578-83-4, name is 1-Bromo-3-methoxy-5-methylbenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a three-necked flask, 3-methyl 5-methoxybromobenzene (8.0 g, 39.8 mmol) was dissolved in tetrahydrofuran (30 mL).Under N2 protection, cool down to -78C, slowly add n-butyllithium (2.6g, 39.8mmol), keep the temperature at -78C, and introduce dioxins.Sulfur gas, reaction 40min. After the reaction was completed, the solvent was distilled off under reduced pressure to give crude 3-methyl 5-methoxybenzenesulfonic acid.

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-Bromo-3-methoxy-5-methylbenzene, 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. 368-21-8, name is 1-(Benzyloxy)-2-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 1-(Benzyloxy)-2-fluorobenzene

O-fluorophenol (5.0 g, 44.6 mmol) was dissolved in tetrahydrofuran (20 mL) was slowly added to tetrahydrofuran (20 mL) suspended in 60% by weight of sodium hydride (2.3 g, 57.5 mmol). After stirring for 5 min, 0.2 mmol of tetrabutylammonium iodide (TBAI) was added and then benzyl bromide (7.3mL, 61.4mmol), a significant exotherm, plus the reaction 0.5h, TLC showed that the raw material has been reacted. The mixture was quenched with saturated aqueous ammonium chloride and extracted with ethyl acetate (2 × 30 mL). The organic phases were combined, dried over anhydrous magnesium sulfate and concentrated to give 11.9 g of the crude product (intermediate A-1a) as a colorless oily liquid. The crude product was dissolved in acetonitrile (50 mL), N-bromosuccinimide (7.3 g, 44.8 mmol) was added and the reaction was carried out at 70 C for 3 h. TLC showed that the starting material had been reacted and most of the acetonitrile was distilled off. 50 mL of water, stirred for 15 min and extracted with ethyl acetate (3 × 30 mL). The combined organic phases were dried over anhydrous magnesium sulfate and purified by column chromatography (pure petroleum ether (PE)) to afford the bromo product (Intermediate A- 2a) as a light yellow oily liquid which solidified to a pale yellow solid (10.5 g, 84% yield). Intermediate A-2a: Murho (singlet): 56-59 C; 6H (300MuEtazeta; CDC13) 7.36-7.7.31 (5H, m), 7.22 (1H, dd, J = 8.1Etazeta, 2.4Etazeta) 7.12 (1H, dt, J = 8.7Hz, 1.8Etazeta), 6.84 (1H, t, J = 8.7Hz), 5.09 (2H, s)

The synthetic route of 368-21-8 has been constantly updated, and we look forward to future research findings.

Related Products of 29578-83-4, A common heterocyclic compound, 29578-83-4, name is 1-Bromo-3-methoxy-5-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.

EXAMPLE 23 SYNTHESIS OF 1-methoxy-3-METHYL-5-[(2E,6E)-3,7,11-TRIMETHYLDODECA-2,6,10-TRIEN-1-YL]BENZENE (24) To a solution of 3-methoxy-5-bromotoluene (0.50 g, 2.49 mmol) in dry THF (8 mL) was added n-BuLi (1.71 mL, 2.74 mmol, 1.6 M in Hexane) dropwise at -78 C. After the reaction mixture was stirred for 15 min, Li2CuCl4 (0.1 mL, 0.1 mmol, 0.1 M in THF) was added, and the mixture was stirred for another 10 min at the same temperature. Then, a solution of (E,E)-farnesyl bromide (0.70 mL, 2.58 mmol) in THF (3 ml) was added over 0.5 hour and stirring was continued for 2 hours at -78 C. After the reaction was complete, the mixture was warmed to room temperature and saturated aqueous NH4Cl (20 mL) was added, followed by 10% NH4OH (40 mL) and Et2O (3 x 50 mL). The combined organic layer was washed with water, brine, and dried with Na2SO4. The crude product was purified by flash silica gel chromatography (hexanes/EtOAc 60:1, 30:1, 20:1 and 10:1) to yield compound 24 (658.1 mg, 78%) as a colorless oil.

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.

These common heterocyclic compound, 6876-00-2, name is 1-Bromo-3-phenoxybenzene, 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. Formula: C12H9BrO

Under an argon atmosphere, butyl lithium (1.56 M, hexane solution: 16 ml) was added at -78C to an anhydrous THF solution (40 ml) of the compound of Reference Example 15 (6.0 g) and stirred at this temperature for 30 minutes. Boric acid triisopropyl ester (4.7 g) was added. The mixture was stirred at -78C for 30 minutes, and after raising the temperature to 25C, the mixture was further stirred for 30 minutes. To the reaction solution, was then added 1 M hydrochloric acid (30 ml), and after 30 minutes of stirring at 25C, the organic layer was separated and washed with saturated brine. The solvent was then evaporated under reduced pressure, thereby giving 4.6 g of the desired product.

The synthetic route of 1-Bromo-3-phenoxybenzene has been constantly updated, and we look forward to future research findings.

Related Products of 458-50-4, These common heterocyclic compound, 458-50-4, name is 4-Bromo-3-fluoroanisole, 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 A1, 1 -dimethylethyl 4-[2~fluoro~4-(methyloxy)phenyl]-3-oxo-1-piperazinecarboxylate A mixture of 1-Boc-3-oxopiperazine (500 mg, 2.497 mmol), 4-bromo-3- fluoroanisole (512 mg, 2.497 mmol), copper(l) iodide (23.78 mg, 0.125 mmol), frans-Nu,Nu’- dimethylcycIohexane-1 ,2-diamine (0.039 mL, 0.250 mmo.), and potassium carbonate (690 mg, 4.99 mmol) in 1 ,4-dioxane (10 mL) was heated at 120 °C for 3.5 days. The mixture was filtered through a pad of Celite and washed with EtOAc (50 mL). The filtrate was washed with saturated aqueous NH4CI (15 mL), brine (15 mL), dried ( gS04), filtered and concentrated. The crude was absorbed on silica gel and purified by silica gelchromatography (10-60percent EtOAc in hexanes) to give 1 ,1 -dimethylethyl 4-[2-fluoro-4- (methyloxy)phenyl]-3-oxo~1 -piperazinecarboxylate (581.9 mg, 1 .794 mmol, 72 percent) as white solid. MS(ESI) m/z: 325.3 (MH+).

Statistics shows that 4-Bromo-3-fluoroanisole is playing an increasingly important role. we look forward to future research findings about 458-50-4.

Application of 332-48-9, A common heterocyclic compound, 332-48-9, name is 1-(2-Bromoethoxy)-4-fluorobenzene, molecular formula is C8H8BrFO, 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 piperazine-1-carboxylic acid /er/-butyl ester (1.86 g, 10 mmol) and l-(2- bromoethoxy)-4-fluorobenzene (2.19 g, 10 mmol) in DMF (5 ml) was added CS2CO3 (7.5 g,20 mmol). The mixture was stirred at room temperature for a day, then quenched with water, and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulphate, and concentrated to yield the title compound quantitatively as an oil (3.25 g) which was used without further purification.1H-NMR (400MHz, DMSO-d6): delta 1.39 (s, 9H), 2.42 (t, 4H), 2.69 (t, 2H), 3.31 (t, 4H), 4.04(t, 2H), 6.95 (m, 2H), 7.10 (t, 2H).

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 51388-20-6,Some common heterocyclic compound, 51388-20-6, name is 4-(Benzyloxy)aniline hydrochloride, molecular formula is C13H14ClNO, 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.

6-(4-Benzyloxyphenylamino)-5-nitronicotinic acid methyl ester (XXIV): To a solution of 6-chloro-5-nitro-nicotinic acid methyl ester (216 mg, 1.0 mmol) and 4-benzyloxyaniline hydrochloride (280 mg, 1.2 mmol) in MeOH (10 mL) was added iPr2NEt (0.35 mL, 2.0 mmol). The resulting mixture was stirred at rt overnight, a red solid precipitated from the mixture, which was collected by filtration. MS (ES, Pos.): m/z 380 [MH+]. 1H NMR (CDCl3, 400 MHz): delta=3.94 (s, 3H), 5.10 (s, 2H), 7.03 (d, J=8.8 Hz, 2H), 7.38-7.46 (m, 5H), 7.50 (d, J=8.8 Hz, 2H), 9.01 (d, J=2.0 Hz, 1H), 9.08 (d, J=2.0 Hz, 1H), 10.2 (br s, 1H).

The synthetic route of 51388-20-6 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., Recommanded Product: 1,3-Dibromo-5-methoxybenzene

A mixture of 3,5-dibromoanisole (10 mmol, 2.7 g)Diphenylamine (60 mmol, 10 g) was added to a 100 mL three-necked flask,A cuprous iodide (6 mmol, 1.2 g) was added under nitrogen,Potassium carbonate (60 mmol, 8.3 g),Phenanthroline (6 mmol, 1.2 g),50 mL of DMF,The reaction was carried out at 155 ° C for 3 days;The resulting reaction product is subjected to extraction,The extracted organic phase was evaporated to dryness with ethanol,Then recrystallized from ethyl acetate and petroleum ether,To give 4.02 g of intermediate C-1,

The synthetic route of 74137-36-3 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. 944317-92-4, name is 1-Bromo-4-fluoro-5-isopropyl-2-methoxybenzene, A new synthetic method of this compound is introduced below., COA of Formula: C10H12BrFO

General procedure: A 500 mL dry flask was charged with 1-bromo-4-fluoro-5-isopropyl-2-methoxybenzene (BrMIP) (24.60 g, 0.10 mol) and dissolved in toluene (80 mL) and THF (80 mL). The resulting solution was flushed with argon, and tri- isopropylborate (32 mL, 0.1 mol) was added. The mixture was cooled to -80 C. Then 2.5 n-BuLi in hexanes (48 mL, 0.12 mol) was added slowly, maintaining a temperature below -55C. After completion of the n-BuLi addition, the reaction mixture was slowly warmed (1 hour) to -10C and water (120 mL) was added, followed by commercially available 2-bromo-5-(trifluoromethyl)benzonitrile (Formula VI’, X = Br, R2 = CN) (25.00 g, 0.10 mmol) and the catalyst, 1 , 1 bis( di-tertbutylphosphino)ferrocene palladium dichloride (265 mg, 0.8 mol%) addition. The organic layer turns dark brown immediately. The biphasic mixture is aged at room temperature with vigorous stirring for 12 hours. The aqueous layer was removed and the organic layer was washed with 1 M NaOH (aq) (100 mL), water (300 mL) and filtered through silica gel. The solvent was removed under reduced pressure to yield brown oil which was crystallized from EtOH/water (300/100 mL). The resulting slurry was filtered and the filter cake was washed with cold 50% EtOH. The product was dried at 40 C under vacuum to yield 4′-fluoro-5′- isopropyl-2′-methoxy-4-(trifluoromethyl)biphenyl-2-carbonitrile (Formula VII’, Ri = CN, R2 = isopropyl) as a pale white solid (25.20 g, 75%). According to the same procedure in various scales and different concentrations of catalyst some other biaryl of Formula Vlh and Vll2 are prepared and listed in Table 3 and Table 4, respectively. For NMR data and melting points see Table 1 and 2.

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.