Category: ethers-buliding-blocks

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. 22807-80-3, name is 1-Bromo-4-(tert-butoxymethyl)benzene, A new synthetic method of this compound is introduced below., Computed Properties of C11H15BrO

(E)-N-(tert-butyl)-2-(4-bromophenyl)-2-oxoacetimidoyl cyanide employs the following steps:1 In a 1000 ml reactor, add 7.29 g of p-bromobenzyl tert-butyl ether, 13.60 ml of t-butyl isocyanide, 0.78 g of silver trifluoromethanesulfonate, and 13.60 g of 2,3-dichloro-5,6-dicyano -1,4-benzoquinone, 300 ml of chlorobenzene, heated to 80 C. The reaction is followed by thin layer chromatography until the reaction material disappears;2 After the reaction is completed, it is cooled to room temperature. The product was extracted with ethyl acetate and washed with saturated brine. After drying, the solvent was removed on a rotary evaporator to obtain a crude product;3 Crude product was purified by column chromatography (peel ether: ethyl acetate = 100:1) to afford 6.24 g of (E)-N-(t-butyl)-2-(4-bromophenyl)-2-oxo Iminoacetyl cyanide having a structural formula of 71%.

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 2982-54-9, These common heterocyclic compound, 2982-54-9, name is 2-(4-(Benzyloxy)phenyl)ethanamine hydrochloride, 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 4. Preparation of 3-((2-(4-benzyloxy-phenyl)-ethylamino)-methyl)-7-methyl-chromen-2-one: 7-Methyl-2-oxo-2H-chromen-3-carbaldehyde (380mg, 2.02mmol) (ScetharamaiyerPadmanabhan, Ravikumar Peri and David J. Triggle, Syn. Comm., 26(4), pp 827-831, 1996) and the compound (130mg, 0.40mmol) prepared in the step 3 were dissolved in dried THF (6ml) and methanol (12ml). thereto triethylamine (0.96ml, 6.87mmol) was added and the reaction mixture was stirred at room temperature for 3 hours. Thereafter, the temperature was lowered to O0C, and thereto acetic acid (0.41ml, 7.07mmol) and sodiumborohydride (0.178mg, 2.83mmol) were added, and the reaction mixture was stirred at O0C for 2 hours. Ice water (0.1ml) was added to quench the reaction, and aqueous layer was extracted with ethyl acetate. Combined organic layer was concentrated under reduced pressure. The residue was purified by column chromatography (n-hexane:ethyl acetate = 1:1) to give 240mg (yield: 29.1%, white solid) of the target compound. 1H-NMR (CDC13, 400MHz) delta 6.79-7.79(m, 13H), 5.05(s, 2H), 4.57(m, IH),2.78-3.54(m, 6H), 2.28(s, 3H)

Statistics shows that 2-(4-(Benzyloxy)phenyl)ethanamine hydrochloride is playing an increasingly important role. we look forward to future research findings about 2982-54-9.

Synthetic Route of 1049730-91-7,Some common heterocyclic compound, 1049730-91-7, name is 2-Bromo-4-methoxy-1-(trifluoromethoxy)benzene, molecular formula is C8H6BrF3O2, 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 stirred solution of 2-Bromo-4-methoxy-1-trifluoromethoxy-benzene (Preparation 59, 19.0 g, 73.9 mmol) in anhydrous tetrahydrofuran (400 ml) was added n-butyl lithium (2.5M solution in hexanes, 44.2 ml, 110.9 mmol) while maintaining the temperature below -7O0C under an atmosphere of nitrogen. The resulting solution was stirred at -7O0C for 1 hour. Tri-/sopropyl borate (20.9 g, 110.9 mmol) was added and the mixture stirred at -7O0C for an additional 2 hours. The reaction mixture was quenched with saturated ammonium chloride aqueous solution (400 ml). The resulting mixture was acidified to pH~5 by addition of hydrochloric acid (1 N aqueous solution). The layers were separated and the organic layer was washed with water (200 ml) then dried over anhydrous MgSO4 (s), filtered and evaporated in vacuo. Residue was purified by recrystallization from ethyl acetate: petroleum ether (2 ml:50 ml) to afford the title compound as a white solid (7.5 g, 43%).1HNMR (c^DMSO): 3.76 (s, 3H), 6.99 (dd, 1 H), 7.06 (d, 1 H), 7.18 (dd, 1 H), 8.36 (s, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-4-methoxy-1-(trifluoromethoxy)benzene, its application will become more common.

Application of 131713-50-3, 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. 131713-50-3, name is 2,2-Dimethoxypropan-1-amine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The precursor 2,2-dimethoxypropylamine can be preparedaccording to the methodology described, for example, in Cui, P.et al., Bioorganic & Medicinal Chemistry Letters, 2006, 16(13),3401-3405. A previously prepared solution of 2,2- dimethoxypropylamine in anhydrous tetrahydrofuran (5.4 g of the amine (41.16 mmol) in 50 mL of the organic solvent) was slowlyadded at a temperature of -5C to the solution obtained according to the methodology described in Comparative Example 6. Once the addition ended, the temperature of the obtained mixture was increased to about 20C, and it was kept under stirring for 16 hours at a temperature of about 20C.Once it no longer had to be kept under the aforementioned conditions, 50 mL of an 8% aqueous NaHCO3 solution and 50 mL of 2-methyltetrahydrofuran were added. The resulting mixture was kept under stirring for about 5 minutes and the resulting organic phase containing (3S)-3-[7-bromo-2-(2,2-dimethoxypropylamino)-5-pyridin-2-yl-3H-benzo[e] [l,4]diazepin-3- yl]propionic acid methyl ester was subsequently separated. The organic solvent was vacuum-distilled, and 50 mL of acetone were added to the resulting residue. The obtained mixture was heated at the reflux temperature and then slowly cooled to about 20C.The resulting solid was filtered and oven-dried, finally obtaining 5.2 g (75.7% from 3-[(3S)-7-bromo-2-oxo-5-(pyridin-2- yl)-2,3-dihydro-1H-[1,4]-benzodiazepin-3-yl] propionic acid methyl ester of formula (D), with a purity of 98.5% by means of UPLC) of (3S)-3-[7-bromo-2-(2,2-dimethoxypropylamino)-5-pyridin- 2-yl-3H-benzo[e] [1,4]diazepin-3-yl]propionic acid methyl ester.Figure 6 shows the 1H-NMR spectrum. 1H-NMR (CDC13, 400 MHz)6 (ppm) : 8.65 (1H, d) , 7.79 (2H, m) , 7.48 (1H, dd) , 7.35 (2H, m)7.10 (1H, d) , 5.18 (1H, m) , 3.70 (3H, s) , 3.64 (1H, dd) , 3.45(1H, dd), 3.31 (1H, dd), 3.22 (3H, s), 3.21 (3H, s), 2.77(1H,m) , 2.65-2.37 (3H, m) , 1.72 (1H, s) , 1.29 (3H, s)Figure 7 shows the 13C-NMR spectrum. 13C-NMR (CDC13, 400MHz) 6(ppm): 173.31, 167.89, 156.77, 154.75, 149.57, 149.16,136.57, 133.78, 133.07, 128.51, 127.10, 124.44, 124.24, 112.33,100.14, 60.24, 51.80, 48.65, 48.62, 45.72, 30.84, 26.23, 20.57.

The synthetic route of 2,2-Dimethoxypropan-1-amine has been constantly updated, and we look forward to future research findings.

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 15799-79-8 as follows. HPLC of Formula: C9H13NO

General procedure: (Scheme 1: cat.= H3PW12O40, oxidant= air, solvent= DMSO/CH3CO2H). A 50mL flask equipped with a magnetic stirrer was charged with 1,4-naphthoquinone (1) (20mmol; 3.16g), aromatic compounds (10mmol), 15mL of CH3COOH and H3PW12O40 (288mg; 1mol%). The flask was heated at 100C for 24h. After that time, the flask was cooled down to room temperature and 15mL of chloroform was added. The solution was washed with 20mL of brine. The organic phase was separated and dried by MgSO4. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel, using a gradient hexane/acetone mixture as eluent.

According to the analysis of related databases, 15799-79-8, the application of this compound in the production field has become more and more popular.

Application of 35202-55-2, 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 35202-55-2 as follows.

Step 2: ethyl (3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl)carbamate 1.5 mL of ethyl chloroformate are poured into a suspension of 3.4 g of the compound obtained in Step 1 in 4.5 mL of triethylamine and 50 mL of dichloromethane and left overnight, whilst stiffing at ambient temperature; washing with water and with 1N hydrochloric acid is then carried out. Drying is carried out and the solvent is evaporated off to dryness. 3.2 g of an oil corresponding to the expected product are obtained. Yield=80%

According to the analysis of related databases, 35202-55-2, the application of this compound in the production field has become more and more popular.

Related Products of 954235-78-0, A common heterocyclic compound, 954235-78-0, name is 4-Bromo-2-(difluoromethoxy)-1-fluorobenzene, molecular formula is C7H4BrF3O, 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.

5-bromo-2-fluoro-1-difluoromethoxybenzene (1.0 g, 4.1 mmol),bis(pinacolato)diboron (1.3 g, 5.0 mmol), 1,1-bis(diphenylphosphino)ferrocene-palladium(II) dichloride dichloromethane complex (0.3 g, 0.4 mmol), KOAc (0.8 g, 8.3 mmol), and anhydrous 1,4-dioxane (8.3 mL) are added to a pressure vessel. Argon is bubbled through the solution for several minutes. The vessel is sealed and is heated at 85 C overnight. After cooling to RT, the reaction mixture is diluted with EtOAc and filtered through diatomaceous earth. The filtrate is concentrated to crude blackish oil under reduced pressure and is dissolved in acetone (14 mL). The resulting suspension is cooled to 0 C and a solution of potassium peroxymonosulfate (3.1 g, 5.0 mmol) in water (13.8 mL) is added over 10 min. After stirring for 2 h while maintaining the temperature at 0C, the reaction mixture is diluted with water (40 mL), and the mixture is extracted with EtOAc (3 x 40 mL). The resulting layers are separated, and the combined organic layers are washed with saturated aqueous NaCl, dried over Na2S04, filtered and concentrated under reduced pressure. The resulting residue is purified by silica gel flash column chromatography, using a gradient of 10-50% EtOAc in hexanes, to yield the title compound (0.77 g, quantitative yield) as a yellow oil. ES/MS m/z 176.8 [M-H].

The synthetic route of 954235-78-0 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 456-55-3, name is (Trifluoromethoxy)benzene, 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 456-55-3, Formula: C7H5F3O

EXAMPLE 1 4-Trifluoromethoxybenzaldehyde (A) with (2-trifluoromethoxybenzaldehyde (B)) 0.5 liter (25 Mol) of HF is added with brine cooling (5 C.) to 162 g (1 mol) of trifluoromethoxybenzene and 140 g (1 mol) of urotropine in a V4 A stainless steel stirred autoclave. The apparatus is sealed pressuretight and heated to 80 C. for 5 hours. A pressure of 6 to 7 bar becomes established. When the reaction has ended, the crude reaction mixture, which is cooled down to 25 C., is stirred into 1 liter of water and stirred therein at 5 C. for 15 minutes, the organic content is then isolated, and the aqueous phase is extracted with methylene chloride. Crude distillation of the washed organic phases gives 135 g of product (boiling point: 72-74 C./8 mbar).

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Reference of 53903-49-4, 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. 53903-49-4, name is 4-Methoxy-2-(trifluoromethyl)aniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(c) 4-Methoxy-6-(methylthiomethyl)-2-(alpha,alpha,alpha-trifluoromethyl)aniline was prepared by substituting 4-methoxy-2-(alpha,alpha,alpha-trifluoromethyl)aniline as follows: In a 250 ml three-necked flask equipped with an overhead stirrer was placed 20.12 g (0.105 mol) of 4-methoxy-2-(alpha,alpha,alpha-trifluoromethyl)aniline in 100 ml of methylene chloride. To the solution was then added 15.63 g (0.117 mol) of N-chlorosuccinimide was added with vigorous stirring. After cooling to 0 C. under a nitrogen atmosphere, a solution of 9.2 ml (8.02 g, 0.129 mol) dimethylsulfide in 40 ml of methylene chloride was then added over a one hour period while maintaining the temperature below 5 C. The reaction mixture became very thick. The ice bath was removed and after stirring at room temperature for one hour, 200 ml of ice cold 5% aqueous sodium hydroxide solution was added. The methylene chloride layer was separated, dried over anhydrous potassium carbonate, filtered and the solvent removed under reduced pressure. To the residue was then added 60 ml of 1,2-dichloroethane and 1.00 g (10 mmol) of succinimide. After refluxing for twelve hours under a nitrogen atmosphere, the reaction mixture was cooled, washed twice with 100 ml of 5% sodium hydroxide solution, dried with magnesium sulfate, filtered and concentrated under reduced pressure to afford 24.9 g of a black oil. This was distilled under reduced pressure to afford 16.5 g (63% yield) of the desired product as a clear, colorless liquid (Bp 106-110 at 0.35 mm Hg) of 95% purity as assayed by gas chromatography; 1 H NMR analysis indicated: (delta, CDCl3) 6.94 (d, J=1.8 Hz, 1H), 6.78 (d, J=1.8 Hz, 1H), 4.32 (br s, 2H, NHz), 3.54 (s, 3H), 3.51 (s, 2H) and 1.82 (s, 3H). Mass spectrum analysis indicated: (m/e) 251 (M+), 204 (100%) and 181.

The synthetic route of 4-Methoxy-2-(trifluoromethyl)aniline has been constantly updated, and we look forward to future research findings.

Application of 126940-10-1, A common heterocyclic compound, 126940-10-1, name is 1-Fluoro-3-(methoxymethoxy)benzene, molecular formula is C8H9FO2, 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: To a flame dried 100mL flask were added 1,3-disustituted benzene (3.0mmol), TMEDA (1.1equiv, 3.3mmol), DIPA (5%equiv, 0.16mmol), and THF (10.0mL). The solution was cooled to -78C for 10min and then n-BuLi (1.1equiv, 3.3mmol) was added dropwise. The mixture was kept at this temperature for 1h; DMF (1.5equiv, 4.5mmol) was added and the mixture was further stirred for another half an hour at -78C. The mixture was allowed to warm up to room temperature and quenched by the addition of saturated NH4Cl-H2O solution (5mL); extracted three times with ethyl acetate (10mL×3). The combined organic layers were dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The regioselectivity of the crude product was ascertained by 19F NMR (for fluorinated products) or by GC/MS (for nonfluorinated ones) and then subjected to flash chromatography to obtain the desired products which were characterized by 1H NMR, 19F NMR, and 13C NMR spectral data and GC-MS analyses.

The synthetic route of 126940-10-1 has been constantly updated, and we look forward to future research findings.