Category: ethers-buliding-blocks

Synthetic Route of 89521-55-1, 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 89521-55-1 as follows.

Example 1 Preparation of 4-benzyloxybenzimidazole STR109 A mixture of 3-benzyloxy-1,2-diaminobenzene 1.6 g (0.0073 mol) and formic acid (2.6 g, 0.057 mol) was heated to reflux for 1.5 h. The resulting mixture was then cooled, dissolved in methylene chloride, washed with 10% sodium carbonate solution, dried (Na2 SO4) and evaporated to dryness in vacuo. The residue was recrystallized from acetonitrile to give the title compound in 0.75 g (46%) yield, m.p. 165-167 C.

According to the analysis of related databases, 89521-55-1, the application of this compound in the production field has become more and more popular.

Related Products of 3616-56-6, These common heterocyclic compound, 3616-56-6, name is 2,2-Diethoxy-N,N-dimethylethanamine, 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.

Synthesis example B6: Synthesis of 12H-benzofuranyl[3,2-a]carbazole (compound 6); (6); Compound 5 (2.8 g, 1 eq.) is added to acetic acid (30 ml) and heated to reflux. (Dimethylamino)acetaldehyde diethyl acetal (95percent; 20.3 g, 10 eq.) is added dropwise in portions to the solution. The reaction is stirred at reflux overnight. Then further (dimethylamino)acetaldehyde diethyl acetal (95percent; 2.0 g) is added and stirred further at reflux after 3 h. Subsequently, the flask contents are diluted with CH2CI2 at room temperature and washed in a separating funnel with distilled water and NaCI (saturated). Organic phase is dried with Na2S04 and concentrated. LC (Si02, 15:85 ethyl acetate/cyclohexane) gives the product 6 (1 .92 g, 62.2percent yield).1 H NMR (CD2CI2, 400 MHz): “5 = 8.88 (br s, 1 H), 8.16 (d, 1 H), 8.12 (d, 2H), 7.66 (d, 1 H), 7.62 (d, 1 H), 7.42-7.53 (m, 4H), 7.31 (dd, 1 H).

The synthetic route of 3616-56-6 has been constantly updated, and we look forward to future research findings.

Electric Literature of 450-88-4, 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. 450-88-4 name is 1-Bromo-4-fluoro-2-methoxybenzene, 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.

EXAMPLE 1; Preparation of 5-(1,3-dihydroisoindol-2-ylcarbonyl)-3-(3-methylbenzyl)-6-hydroxy-1H-indazole (?A1?); 1.1; 12 ml of dichloromethane are added to 3.25 g of aluminium chloride under argon, and the mixture is cooled to -55 C. with stirring. A solution of 2.5 g of 2-bromo-5-fluoroanisole and 2.47 g of m-tolylacetyl chloride in 8 ml of dichloromethane is added dropwise at this temperature. The mixture is stirred for a further 10 minutes, allowed to warm slowly to 0 C. and subsequently hydrolysed using 1N HCl. The mixture is stirred for a further 15 minutes, diluted with dichloromethane and subjected to conventional work-up. The residue obtained is digested with petroleum ether/diethyl:ether (8:2), filtered off with suction and rinsed with petroleum ether. Drying gives 1.85 g of ?1a?

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

Application of 352-67-0, 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. 352-67-0, name is 1-Fluoro-4-(trifluoromethoxy)benzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A. 1 -Fluoro-2-nitro-4-trifluoromethoxy-benzene and 4-Fluoro-2-nitro-1 – trifluoromethoxy-benzeneTo a mixture of 1-fluoro-4-trifluoromethoxy-benzene (31.57 g, 0.18 mol) in cone. H2SO4 (100 ml_) at 0C is added cone. HNO3 (30 ml_) dropwise over a 10 min period. After the mixture is stirred at 0 C for 1 h, it was poured into ice. The mixture is extracted with EtOAc. The organic extract is washed with H2O (3x) and brine, dried over MgSO4, filtered, and concentrated in vacuo to yield 38 g (96%) of the product as a mixture of 1 -fluoro-2-nitro-4-trifluoromethoxy-benzene and 4-fluoro-2-nitro-1 – trifluoromethoxy-benzene (-30/70, based upon 19F NMR). 1H NMR (CDCI3): delta 8.00- 7.90 and 7.80-7.65 (m, 1 H), 7.60-7.25 (m, 2H); 19 F NMR (CDCI3) delta -57.59 and -58.11 (s, 3F), -109.07 and -117.90 (t, J = 6.2 and d, J = 6.2, 1 F).B. 2-Fluoro-5-trifluoromethoxy-phenylamine and 5-Fluoro-2-trifluoromethoxy- phenvlamine A mixture of 1 -fluoro-2-nitro-4-trifluoromethoxy-benzene and 4-fluoro-2-nitro-1 – trifluoromethoxy-benzene and Raney Ni (2800) in MeOH (250 ml_) is hydrogenated at 40 psi for 5 h (or until no more H2 is consumed). The catalyst is filtered off, and the filtrate is concentrated in vacuo. The residue is redissolved in CH2CI2, dried over MgSO4, filtered, and concentrated in vacuo to yield 27.4 g of the product (dark brown liquid) as a mixture of 2-fluoro-5-trifluoromethoxy-phenylamine and 5-fluoro-2- trifluoromethoxy-phenylamine (-30/70, based upon 19F NMR). 1H NMR (CDCI3): delta 7.15-6.90 (m, 1 H), 6.70-6.30 (m, 2H), 3.60-4.25 (br m, 1 H); 19 F NMR (CDCI3) delta -57.77 and -57.86 (s, 3F), -113.83 and -137.09 (1 H); MS 196 (M+1 , 100%).

The synthetic route of 1-Fluoro-4-(trifluoromethoxy)benzene has been constantly updated, and we look forward to future research findings.

Synthetic Route of 5414-19-7, These common heterocyclic compound, 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, 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 the product of Part E (6.8 g, 15.5 mmol), potassium carbonate (Aldrich, 7.5 g, 54.3 mmol), and 18-crown-6 (Aldrich, 0.5 g, cat. amt) in N,N-dimethylformamide (30 ml) was added dibromo-diethylether (Aldrich,2.9 ml, 23.2 mmol). The mixture was heated at 60 C. for 18 hr, and then worked up by cooling and pouring into water (50 ml). The mixture was extracted via ethylacetate (2?-150 ml). The organics were combined and washed with 5% HClaq (1?-50 ml), water (1?-100 ml), and brine (2?-100 ml); dried over Na2SO4; and concentrated to afford a yellow oil that solidified. The solid was recrystallized from methanol to produce the desired compound in the form of a white solid (4.8 g, 76% yield). 1H NMR was consistent with the desired structure.

The synthetic route of 5414-19-7 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. 3401-47-6, name is 1-Bromo-2-methoxynaphthalene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 3401-47-6

General procedure: An oven-dried vial (35×12 mm) equipped with a PTFE-sealedxscrew cap was loaded with a magnetic stirrer bar, ((+/-)-binap)Ni[P(OPh)3]2*2PhCH3 (9) (39 mg, 25 mmol, 5mol-%), (+/-)-binap (15 mg, 25 mmol, 5 mol-%), and the corresponding aryl halide (0.50 mmol, 1.0 equiv.). The vial was then transferred into an argon-filled glovebox, where NaOtBu (216 mg, 2.20 mmol, 4.40 equiv.) and NH3 (0.5 M in 1,4-dioxane, 3.0 mL, 1.5 mmol, 3.0 equiv.) were added. The reaction vial was capped, removed from the glovebox, and placed into a preheated oil bath at 120 C to stir for 18 h. On cooling, the reaction mixture was diluted with Et2O (15 mL), and washed with 1 M NaOH (10 mL) and H2O (210 mL). The organic layer was fused onto silica and purified via flash column chromatography (EtOAc/hexanes or EtOAc/MeOH) to give the corresponding aniline. 2-Methoxynaphthalen-1-amine (19l) Following the general procedure using 1-bromo-2-methoxynaphthalene (119 mg, 0.500 mmol), the desired compound 19l was obtained after purification via flash column chromatography(hexanes/EtOAc 90 : 10) as a dark-orange oil (62 mg, 0.36 mmol, 72 %). The spectral data were in accordance with those reported in the literature.[65] Rf 0.22 (hexanes/EtOAc 90 : 10). deltaH (CDCl3, 500 MHz) 7.80-7.77 (2H, m, 2Ar-H), 7.46-7.42 (1H, m, Ar-H), 7.38-7.33 (2H, m, 2Ar-H), 7.26 (1H, d, J 8.8, Ar-H), 4.23 (2H, br s, NH2), 3.98 (3H, s, OMe). deltaC (CDCl3, 125 MHz) 142.6 (Ar-C), 129.6 (Ar-C), 129.5 (Ar-C), 128.5 (Ar-CH), 125.1 (Ar-CH), 124.0 (Ar-C), 123.7 (Ar-CH), 120.4 (Ar-CH), 118.5 (Ar-CH), 113.7 (Ar-CH), 56.8 (OMe).

The synthetic route of 3401-47-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 7664-66-6, 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. 7664-66-6, name is 4-Isopropoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The compound obtained in Step 3 (60 mg) was dissolved in acetonitrile (1.5 mL), 4-isopropoxy aniline (40 mg) was added and stirred for 30 minutes under microwave irradiation under 180 C. It extracted three times with chloroform. After addition of a saturated aqueous sodium hydrogen carbonate solution to the reaction solution. Then, the organic layer was concentrated and dried over sodium sulfate. The resulting residue to give the title compound purified by silica gel column chromatography (82mg, 100%).

The synthetic route of 4-Isopropoxyaniline has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 658-89-9, name is 4-(Trifluoromethoxy)benzene-1,2-diamine, molecular formula is C7H7F3N2O, 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. COA of Formula: C7H7F3N2O

A mixture of S-bromo-lH-pyrazoloP^-bjpyridine-S-carboxyric acid Compound Ic (0.68 g, 1.93 mmol), Compound 16b (0.373 g, 1.93 mmol), HATU (0.73 g, 1.9 mmol) and DIPEA (1 mL, 5.8 mmol) in DMF (30 mL) was stirred at room temperature overnight. The solvent was removed under vacuum and the resulting yellow residue was mixed with AcOEt, sequentially washed with saturated aqueous NH4Cl, IM HCl, water and saturated aqueous NaHCO3, then dried over Na2SO4. The solvent was evaporated to dryness to provide 5-bromo-lH-pyrazolo[3,4-b]pyridine-3- carboxylic acid (2-amino-4-trifluoromethoxy-phenyl)-amide Compound 16c (0.67 g, 83% yield) as a yellow solid. LC-MS major peak 3.03 min, MS (ESI) m/z 416.0 (M+)/417.0 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 658-89-9, its application will become more common.

Electric Literature of 4316-51-2, A common heterocyclic compound, 4316-51-2, name is 4-Methoxytriphenylamine, molecular formula is C19H17NO, 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.

Boron tribromide was added to a dichloromethane solution of 4-methoxytriphenylamine (formula (6)) while cooling, and the mixture was stirred at room temperature for 3 hours to obtain diphenylaminophenol (formula (7) in a yield of 90% It was.

The synthetic route of 4316-51-2 has been constantly updated, and we look forward to future research findings.

Application of 102-52-3, 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 102-52-3 as follows.

Preparation of 5-(3-methoxy-4-(1H-pyrazol-1-yl)phenyl)oxazole (IIe) To a suspension of intermediate IId (1.834 g, 8.94 mmol) in EtOH (30 ml) were added malonaldehyde bis(dimethyl acetal) (1.63 ml, 9.84 mmol) and conc.HCl (1 ml). The reaction mixture was stirred at 70 C. for 2 hours. The cooled mixture was evaporated to dryness, diluted saturated solution of NaHCO3 and extracted with EtOAc twice. The combined organics were washed with water, with saturated solution of NaCl, dried over MgSO4, filtered and evaporated. The final product was purified by silica gel chromatography using 0 to 30% EtOAc/cyclohexane as eluent to give intermediate IIe (1.380 g, 64%). 1H NMR (500 MHz, CDCl3) delta 8.12 (d, J=2.1 Hz, 1H), 7.94 (s, 1H), 7.85 (d, J=8.3 Hz, 1H), 7.72 (d, J=1.4 Hz, 1H), 7.40 (s, 1H), 7.36 (dd, J=8.3, 1.8 Hz, 1H), 7.32 (d, J=1.7 Hz, 1H), 6.46-6.43 (m, 1H), 3.97 (s, 3H).

According to the analysis of related databases, 102-52-3, the application of this compound in the production field has become more and more popular.