Month: May 2021

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.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 1535-75-7 as follows. Computed Properties of C7H6F3NO

General procedure: A mixture of B (1 mmol) and dichloromethane (10 ml) was stirred for 10 min, then EDCI (1.2 mmol) and HOBt (1.2 mmol) were added. Added the appropriate amine (1.2 mmol) into the mixed solution after 30 min and refluxed for 12 h. The reaction mixture was filtrated with water and then the filtrate was dried and evaporated. Purification by silica gel afforded C1-C27

According to the analysis of related databases, 1535-75-7, the application of this compound in the production field has become more and more popular.

Application of 2050-46-6, 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. 2050-46-6 name is 1,2-Diethoxybenzene, 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.

18.9 g of 1,2-diethoxybenzene obtained in Production Example 9 and 22.0 g of 3-bromobenzoyl chloride were dissolved in 100 ml dichloromethane, and 100 ml of 1.0 M tin tetrachloride in dichloromethane was added dropwise thereto under ice-cooling. After the dropwise addition, the mixture was further stirred at room temperature for 15 hours. The reaction solution was poured into ice-cold water to terminate the reaction, and the organic layer was recovered, washed with water twice and with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was recrystallized from hexane-ethyl acetate to give 23.8 g of the title compound as colorless crystals. 1H-NMR (400 MHz, CDCl3) delta 1.46-1.52 (6H, m), 4.13-4.21 (4H, m), 6.89 (1H, d, J=8.8 Hz), 7.32 (1H, dd, J=8.8,2.0 Hz), 7.35 (1H, t, J=7.8 Hz), 7.46 (1H, d, J=2.0 Hz), 7.64-7.71 (2H, m), 7.88 (1H, t, J=l.6 Hz).

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

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. 6298-96-0, name is 1-(4-Methoxyphenyl)ethylamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 6298-96-0

A solution of (S)-(-)-1-(4-methoxyphenyl)ethylamine (25.0 g, 166 mmol) and 6,7-dihydro-8(5W)-quinolinone (24.0 g, 166 mmol, J. Org. Chem., 2002, 67, 2197-2205) in dichloromethane was treated with glacial acetic acid (14.0 mL, 249 mmol) and sodium triacetoxyborohydride (53.0 g, 249 mmol). The reaction mixture was stirred at room temperature for 15 hours and then treated with sodium carbonate (106 g, 996 mmol) dissolved in water. The resulting mixture was stirred for 30 minutes and then diluted with dichloromethane. The phases were separated and the aqueous solution extracted with an additional portion of dichloromethane. The combinedorganic solutions were dried over MgS04 and concentrated to dryness at reduced pressure. The crude product was purified by flash chromatography (silica gel, gradient elution of dichloromethane to 97:3 dichloromethane/2M ammonia in MeOH) followed by recrystallization from hexane to afford 33 g (70%) of (8S)-/V-{(1S)-1-[4-(methyloxy)phenyl]ethyl}-5,6,7,8-tetrahydro-8-quinolinamine as a white crystalline solid. 1H-NMR (CDCI3): 8 8.40 (m, 1H), 7.33 (m, 3H), 7.04 (m, 1H), 6.84 (d, 2H), 4.02 (m, 1H), 3.83-3.78 (m, 4H), 2.73-2.62 (m, 2H), 1.82 (m, 1H), 1.72 (m, 1H), 1.57 (m, 2H), 1.43 (d, 3H).

The synthetic route of 6298-96-0 has been constantly updated, and we look forward to future research findings.

Application of 7252-83-7, A common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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.

2-[3,6-Bis-(2,2-dimethoxy-ethoxy)-2,7-difluoro-9H-xanthen-9-yl]-benzoic acid 2,2-dimethoxy-ethyl ester (Compound 102) Acid 101 (all material prepared in the previous step, ~10.9 mmol) was dissolved in 150 mL of DMF. Powdered K2CO3 (25 g, 180 mmol) was added to the solution followed by adding of bromoacetaldehyde dimethyl acetal (33.3. mL, 283 mmol). The reaction mixture was stirred overnight at 110 C. DMF solution was removed from the flask (leaving insoluble material in the flask) and evaporated. The residue was mixed with 150 mL of water and combined with the solid left in the flask. The product was extracted with ethyl acetate (4*45 mL), combined extracts were washed with water (4*30 mL), brine (30 mL), dried over sodium sulfate and evaporated in vacuum. The residue was dissolved in chloroform, loaded on silica gel column (packed in 100:3 chloroform-EtOAc mixture). The column was eluted with 100:3 chloroform-EtOAc mixture. Pure fractions containing the product were combined and evaporated to give ester 102 as a clear oil, solidified later to form white solid (4.54 g, 66%).

The synthetic route of 7252-83-7 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. 2930-05-4, name is 2-((Benzyloxy)methyl)oxirane, This compound has unique chemical properties. The synthetic route is as follows., name: 2-((Benzyloxy)methyl)oxirane

General procedure: To a CO2 balloon equipped 10 mL round-bottomed flask containing indium bromide (0.178 g, 0.5 mmol) was added triphenylphosphine (0.262 g, 1 mmol) at rt. Epoxide 1 (10 mmol) was added, and stirred at rt for 5 h. The reaction system is gas (CO2)-liquid (substrate) biphasic system. To the reaction mixture was added 10 mL of H2O. The mixture was extracted with Et2O (10 mL) for three times. The organic layer was dried over MgSO4. After filtration and evaporation, the corresponding carbonate 2 was obtained in almost pure form. Yield was determined by comparing the ratio of product to substrate in the 1H NMR spectrum of the crude mixture. CAS Nos. 2a: 40492-31-7, 2b: 108-32-7, 2c: 66675-43-2, 2d: 4427-92-3, 2e: 4427-96-7, 2f: 2463-45-8, 2g: 949-97-3, 2h: 13818-44-5. For example, spectral data for 2a: Purification was done by distillation under reduced pressure. bp 85 C/0.07 mm Hg; IR (neat) 2900, 1789, 1172 cm-1; 1H NMR (CDCl3) delta 3.43 (s, 3H, OCH3), 3.54 (dd, 1H, J = 3.9 and 11.2 Hz, one of MeOCH2), 3.67 (dd, 1H, J = 3.4 and 11.2 Hz, one of MeOCH2), 4.37 (dd, 1H, J = 6.3 and 8.3 Hz, one of OCH2), 4.51 (t, J= 8.3 Hz, 1H, one of OCH2), 4.80-4.88 (m, 1H, OCH); 13C NMR (CDCl3) delta 59.3, 66.0, 71.3, 75.0, 154.9; EIHRMS calcd for C5H8O4 132.0423, found 132.0420.

According to the analysis of related databases, 2930-05-4, the application of this compound in the production field has become more and more popular.

Related Products of 707-07-3, 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. 707-07-3, name is (Trimethoxymethyl)benzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 18 (1.03 g, 1.77 mmol) was dissolved in dry N,N-dimethylformamide (2 ml) and trimethylorthobenzoate (1.2 ml, 7.08 mmol). The solution was stirred under vacuum (ca 10 mbar) for 10 min then d(+)-camphorsulfonic acid (0.020 g, 0.088 mmol) was added. The mixture was stirred under vacuum for 3 h then triethylamine (0.5 ml) was added and the reaction mixture was concentrated. The residue was dissolved in CH2Cl2, washed with water then the aqueous layer was extracted with CH2Cl2. The combined organic layers were dried (MgSO4), filtered and concentrated.The crude residue was dissolved in dry THF (5 ml) containing n-tetrabutylammonium fluoride (1.67 g, 3.09 mmol). The mixture was stirred at room temperature for 3 h then concentrated. The residue was taken up in CH2Cl2, washed with brine then the aqueous layer was extracted with CH2Cl2. The combined organic layers were dried (MgSO4), filtered and concentrated.To a solution of the previous residue in dry N,N-dimethylformamide (10 ml) was added benzyl bromide (0.65 ml, 3.09 mmol) under argon. The solution was cooled to 0 C then sodium hydride (0.250 g, 3.60 mmol) was added portionwise. The mixture was stirred at room temperature overnight then methanol was added and concentrated. The residue was dissolved in CH2Cl2, washed with brine then the aqueous layer was extracted with CH2Cl2. The combined organic layers were dried (MgSO4), filtered and concentrated.The residue was dissolved in a mixture of THF (5 ml), acetic acid (4 ml) and water (1 ml) and stirred at room temperature for 2 h. The solution was diluted with CH2Cl2 then washed with satd aq NaHCO3. The aqueous layer was extracted with CH2Cl2 then the combined organic layers were dried (MgSO4), filtered and concentrated.

The synthetic route of (Trimethoxymethyl)benzene has been constantly updated, and we look forward to future research findings.

Electric Literature of 101-84-8, These common heterocyclic compound, 101-84-8, name is Diphenyl oxide, 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 3; Preparation of Partially brominated DPO[0050] To the 500 mL 4-neck flask equipped as in Example 2 was added 732g of Br2. Molten diphenyl oxide (49.3 g) was added dropwise at bromine reflux over 40 minutes. The solution was refluxed (O0C condenser) 45 minutes longer. Catalyzed Bromination[0051] To the 1-liter flask, equipped as in Example 2, were added 4.0 g of AlCl3 and 595 g of bromine. This mixture was brought to reflux through the fractionation column and the contents of the 500 mL flask were pumped in at -0.5 niL/min via the 1/16″ (ca. 0.16 cm) O. D., 1/32″ (ca. 0.08 cm) LD. diptube subsurface to the resulting reaction mass. The reaction mass temperature was 590C. The reaction mass was kept at hard reflux throughout the solution addition. The temperature of the cooling water on condenser was 170C. Eight hours later, all of the contents of the 500 mL flask had been pumped into the 1 -liter flask. About 5 mL of bromine was added to the 500 mL flask and this bromine was pumped into the 1 -liter flask. The reaction mass was then refluxed 15 minutes longer with a N2 purge (about 100-200 niL/min. down the diptube). The reaction mass was cooled partially, and 50O mL of H2O was added and the reactor was set for distillation. Bromine was distilled to 1000C and the reaction mass was cooled to 6O0C. Excess 5% NaOH added to pH 12. The solid product was collected and washed well with H2O. A sample was analyzed by GC. GC analysis showed the product to contain 0.017% of the first nonabromodiphenyl oxide peak (meta and para isomers), 0.031% of the second nonabromodiphenyl oxide peak (ortho isomer) and 99.95% of decabromodiphenyl oxide. The remainder of the product was dried overnight at 13O0C and, after drying, weighed 263 g. EXAMPLE 4; Preparation of Partially brominated DPO [0052] To 50.0 g of DPO in a 500 rnL flask equipped with magnetic stirrer, addition funnel, thermometer, and condenser was added 29 g of bromine dropwise over 30 minutes. The reactor was cooled in a water bath. When all the bromine had been added, the reactor was purged with nitrogen to facilitate pumping and prevent HBr breakout in the line. Catalyzed Bromination [0053] In a 1-liter 4-neck Morton flask were placed 4.05 g of AlCl3 and 1230 g of bromine.The flask was equipped with 1/32-inch (ca. 0.08 cm) LD. diptube (subsurface) and a fractionation column as described in Example 2 and topped with a tap water cooled Friedrich condenser. This mixture was brought to reflux and the DPO mixture was pumped into the reactor via the 1/32-inch diptube. Reaction temperature was 590C. Heating was such that bromine vapor rose to about 1A of the height of the condenser before totally condensing. The temperature of the cooling water exiting the condenser was 25.6C. After 6 hours and 58 minutes of feeding, all of the DPO had been added except for about Ig remaining in the flask. The diptube was removed and the reaction mixture was refluxed 10 minutes longer. Water (500 mL) was added and the reactor was set for bromine distillation. Bromine was distilled to a reaction temperature of 1000C. 658 g of bromine was collected. The reactor was cooled,5% NaOH was added to pH of about 13, and the product was collected and washed. GC analysis showed the product to contain 0.020% of the first nonabromodiphenyl oxide peak (meta and para isomers), 0.080% of the second nonabromodiphenyl oxide peak (ortho isomer) and 99.90% of decabromodiphenyl oxide. The product was dried overnight at 1300C. After drying overnight the product weighed 265.2 g. EXAMPLE 5Preparation of Partially brominated DPO[0054] To the 500 mL flask (equipped as described in Example 4) containing 51.67 g ofDPO was added 30.0 g of bromine over about 10 minutes with cooling in a water bath. After stirring for 15 minutes this mixture was nitrogen sparged to remove HBr.Catalyzed Bromination[0055] In a 1 -liter jacketed 4-neck flask equipped with a thermocouple, 1/32-inch LD. dip tube, mechanical stirrer and 9 inch x 1 inch (ca. 22.8 cm x 2.54 cm) column (packed with 5 mm x 5 mm Raschig rings) and topped with a water-cooled Friedrich condenser, and heated by circulating hot water through the jacket, the water temperature being controlled to give the desire reaction temperature, were placed 4.0 g OfAlCl3 and 1240 g of bromine. This mixture was heated to 56.70C and DPO addition initiated. After a DPO feed time of 9 hours and 42 minutes, during which time the reaction temperature was maintained mainly at 56.10C to 57.10C, the feed was stopped and the mixture was refluxed 5 minutes longer under a nitrogen purge of the reaction flask. Then 500 mL of water was added and the flask was set for distillation. 617 Grams of bromine was distilled to a temperature of 800C. The stirrer in the flask was stopped and the resultant water phase was decanted. The solids were washed with 500 mL of water and the water was decanted. Then 500 mL of water and 10 g of NaOH were added to the solids and the mixture …

The synthetic route of 101-84-8 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. 102-52-3, name is 1,1,3,3-Tetramethoxypropane belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1,1,3,3-Tetramethoxypropane

a) Add 2 mol of 1,1,3,3-tetramethoxypropane to the reaction vessel at room temperature and add under stirring0.4 mol mass fraction of 12% hydrochloric acid, the reaction temperature was controlled at 40 C., and the reaction was stirred for 2 h.

The synthetic route of 102-52-3 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. 26510-91-8, name is 2,4,5-Trimethoxyaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 2,4,5-Trimethoxyaniline

Sodium (0.26 g, 11.5 mmol) is added in small portions to MeOH (25 mL). The solution of NaOMe is added to 4-chloro-2,5-dimethoxynitrobenzene (2.27 g, 10.4 mmol) in MeOH (50 mL) at 0 C. The reaction is refluxed for 48 h, cooled to RT and quenched with 1M citric acid (50 mL) and H2O (50 mL). The MeOH is removed under reduced pressure and the aqueous is extracted with EtOAc (3×50 mL), dried (MgSO4), and the solvent is removed. The product is purified by Biotage Flash Chromatography (40M) using 30% EtOAc:hexanes as the eluent to give starting material (1.41 g) and 2,4,5-trimethoxynitrobenzene (0.80 g, 95% based on recovered starting material) as a yellow solid. 2,4,5-Trimethoxynitrobenzene (0.44 g, 2.1 mmol) is dissolved in minimal EtOAc (5 mL) and diluted with EtOH (50 mL). 10% Pd/C catalyst is added as a slurry in EtOAc and the mixture put on the Parr apparatus in the presence of H2 (45 psi to 33 psi) for 0.5 h. The reaction mixture is filtered over celite to remove the catalyst and the solvent is removed to give 2,4,5-trimethoxyaniline (0.34 g, 86% yield) as a light pink solid. 2,4,5-Trimethoxyaniline (0.33 g, 1.8 mmol) is added dropwise as a solution in EtOAc (25 mL) to phosgene (7.6 mL, 20% in toluene) in EtOAc (50 mL). After complete addition, the reaction is heated under reflux for 0.5 h. The reaction is cooled to RT and the solvent is removed under reduced pressure to give 1-isocyanato-2,4,5-trimethoxybenzene (0.37 g, 99% yield) as a light brown solid. Example 143 is obtained using the isocyanate according to Method A making non-critical variations. Yield 44%. HRMS calcd for C13H13F3N4O4S+H 379.0688 found 379.0695.

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.