Author: Jessica.F

Related Products of 7252-83-7, 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 7252-83-7 as follows.

4-Hydroxythiobenzamide (0.20 mol) and 2-bromo-1,1-dimethoxyethane (0.20 mol) were stirred in ethanol (600 mL) at room temperature and p-toluenesulfonic acid (0.20 mol) was added. Into the reaction solution. Heat to 90 C for 24 h. After the reaction was completed, it was cooled to room temperature, and the solvent was evaporated under reduced pressure, and water (200 mL) was added.The pH was adjusted to 8 with saturated sodium bicarbonate solution, extracted with dichloromethane (200 mL¡Á3), and the organic phases were combined.Concentration under reduced pressure and distillation gave 2-(4-hydroxyphenyl)thiazole.

According to the analysis of related databases, 7252-83-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ocean University of China; Shao Changlun; (69 pag.)CN108658937; (2018); A;,
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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. 3586-14-9, name is 1-Methyl-3-phenoxybenzene, A new synthetic method of this compound is introduced below., COA of Formula: C13H12O

EXAMPLE 1 Into a 200 ml four necked flask equipped with a distillation column, 36.9 g (0.2 mole) of m-phenoxytoluene and 1.0 g of powdery activated carbon were charged and heated at 180 C. while stirring and then, 71.1 g of 1,2-dibromotrichloroethane (0.24 mole) was added dropwise for 30 minutes and the reaction was continued at the temperature for 3 hours. After the reaction, the reaction mixture was analyzed by a gas chromatography, 1,2-dibromotrichloroethane disappeared, and the production of 27.5 g of m-phenoxybenzyl bromide and 20.2 g of m-phenoxybenzylidene dibromide were found.

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.

Reference:
Patent; Toyo Soda Manufacturing Co., Ltd.; US4393246; (1983); A;,
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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. 621-23-8, name is 1,3,5-Trimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1,3,5-Trimethoxybenzene

In the reactor, 100 mg of 1,3,5-trimethoxybenzene and 20 mg of boron-nitrogen carbon photocatalyst were added.100 mg of ammonium chloride is an amine source, 3 ml of dimethyl sulfoxide and 1.2 equivalents of cesium fluoride (regulating the pH of the initial reaction solution to 8-10),The reaction was stirred with light at room temperature for 48 h in an oxygen atmosphere, and then extracted with ethyl acetate.The combined organic layers were dried, filtered and evaporatedThe column chromatography eluate used was a petroleum ether: ethyl acetate mixed solvent in a volume ratio of 10:1.The yield was 41%.

According to the analysis of related databases, 621-23-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fuzhou University; Wang Xinchen; Zheng Meifang; Yuan Tao; Shi Jiale; (7 pag.)CN108546233; (2018); A;,
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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. 532440-88-3, name is 2-Bromo-5-methoxy-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Bromo-5-methoxy-4-methylaniline

f. N-(2-bromo-5-methoxy-4-methyl-phenyl)-isobutyramide. To a biphasic mixture of 2-bromo-5-methoxy-4-methyl-aniline (5.6 g, 25.96 mmol), 10% KOH (27 mL) and dichloromethane (30 mL), was added dropwise isobutyryl chloride (3 mL, 28.55 mmol) in dichloromethane (10 mL). The reaction mixture was stirred at room temperature for 48 hrs. The layers were separated. The aqueous layer was further extracted with dichloromethane and the combined organics washed successively with water and brine, dried over MgSO4, filtered and evaporated to give 7.38 g of N-(2-bromo-5-methoxy-4-methyl-phenyl)-isobutyramide (99% yield). 1H NMR (300 MHz; CDCl3): 1.29 (d, J=6.9 Hz, 6 H), 2.14 (s, 3 H), 2.59 (m, 1 H), 3.84 (s, 3 H), 7.24 (s, 1 H), 7.66 (br s, 1 H), 8.07 (s, 1 H).

According to the analysis of related databases, 532440-88-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfahl, Magnus; Tachdjian, Catherine; Spruce, Lyle W.; Al-Shamma, Hussien A.; Boudjelal, Mohamed; Fanjul, Andrea N.; Wiemann, Torsten R.; Pleynet, David P.M.; US2003/144329; (2003); A1;,
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Reference of 801282-00-8, These common heterocyclic compound, 801282-00-8, name is 2-Fluoro-3-methoxyaniline, 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.

00157] Preparation of compound 10[00158] To a solution of compound 9 (13 g, 92 mmol) in DMF (100 mL) was added a solution of NBS (16.4 g, 92 mmol, 1.0 eq) in DMF (100 mL) drop-wise. The reaction mixture was stirred at room temperature for 3h, then diluted with ethyl acetate (500 mL) and washed with brine (2xl50mL). The organic phase was dried (Na2S04), filtered and concentrated to give the title compound 10 as brown oil (23 g, 98% yield). ESI-MS (M+H) : 219.9.

Statistics shows that 2-Fluoro-3-methoxyaniline is playing an increasingly important role. we look forward to future research findings about 801282-00-8.

Reference:
Patent; SUZHOU KINTOR PHARMACEUTICALS,INC.; TONG, Youzhi; WO2012/119559; (2012); A1;,
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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 456-49-5 as follows. Recommanded Product: 1-Fluoro-3-methoxybenzene

To a solution of n-butyllithium (2.6 M, n-hexane solution, 12.7 mL, 33 mmol) dissolved in THF (100 mL) was addeddropwise a solution of 3-fluoroanisole (3.44 mL, 31.1 mmol) dissolved in THF (10 mL) at -78 C. After stirring for 10min at the same temperature, to the mixture was added dropwise a solution of iodine (9.14 g, 36.0 mmol) dissolved inTHF (60 mL) at -78 C. After stirring for 30 min at the same temperature, to the mixture were added aqueous saturatedammonium chloride (20 mL) and then aqueous saturated sodium thiosulfate (40 mL). The mixture was extracted withn-hexane (20 mL ¡Á 3), and the combined organic extract was washed with brine (20 mL), dried (Na2SO4), and afterfiltration, the filtrate was concentrated under reduced pressure. The residue was purified by flash columnchromatography (silica-gel 156 g, n-hexane/EtOAc = 5/1) to give 3-fluoro-2-iodoanisole (7.03 g, 27.9 mmol, 93.0%) asa colorless oil.

According to the analysis of related databases, 456-49-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Yoshida, Suguru; Nagai, Akira; Uchida, Keisuke; Hosoya, Takamitsu; Chemistry Letters; vol. 46; 5; (2017); p. 733 – 736;,
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Reference of 458-03-7, A common heterocyclic compound, 458-03-7, name is 1-Ethoxy-3-fluorobenzene, molecular formula is C8H9FO, 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-Ethoxy-phenyl)-2-methyl-propionitrile was prepared using a procedure adapted from literature (Organic Syntheses, Vol. 79, pp. 209-215). To a solution of 1-ethoxy-3-fluoro benzene (3.0 g, 19.4 mmol) in 25 mL of toluene was added solid potassium bis (trimethylsilyl)amide (5.84g, 29.2 mmol, 1.5 eq) followed by isobutyronitrile (7.08 mL, 77.8 mmol, 4 eq). The reaction mixture was stirred at 100 C for 12 hr. It was diluted with 75 mL of ethyl acetate and 75 mL of IN aqueous hydrochloric acid. The layers were separated, and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with water (1 x 50 mL), brine (1 x 50 mL), and dried over anhydrous magnesium sulfate. The solids were filtered off, and the filtrate was concentrated in vacuo. The residue was dissolved in 5 mL of methylene chloride and applied to a 40 g silica gel cartridge. The product was eluted using a gradient of ethyl acetate in hexanes to yield 2.96 g (15.6mmol, 80%) of pure 2-(3-ethoxy- phenyl) -2-methyl-propionitrile. LR-MS: 190.12 [(M+H)+] 2- (3-Ethoxy-phenyl)-2-methyl-propionitrile (2.96 grams, 15.65 mmol) was dissolved in a freshly prepared acetic acid solution of iodine monochloride (20 mL of a 1.54 M iodine monochloride solution in acetic acid, 30.8 mmol). The reaction was slightly exothermic. The reaction mixture was allowed to stand at room temperature for 3 d. The reaction mixture was concentrated, and the residue was partitioned between ethyl acetate and water. The organic layer was washed with 10% sodium carbonate (1x), brine (1x), and dried (anhydrous magnesium sulfate). The solids were filtered off, and the filtrate was concentrated to dryness. The residue was purified by flash chromatography (110 g of silica gel, eluting with a gradient of ethyl acetate in hexanes) to give 2- (3-ethoxy-4-iodo-phenyl)-2-methyl-propionitrile g, 51%). LR-MS: 316.21 [(M+H)+] Nitrogen gas was bubbled through a solution of (3-ethoxy-4-iodo-phenyl)-2-methyl- propionitrile (2.53 grams, 8 mmol) and diisopropylethylamine (2.09 mL, 12 mmol) in methanol (10 mL). Using a balloon filled with carbon monoxide gas (CO) and equipped with a needle, CO was bubbled through the mixture until it was saturated. Palladium (II) acetate (100 mg) was added, and the mixture was stirred under an atmosphere of CO at 60 C for 6 d. The reaction mixture was filtered and concentrated. The residue was partitioned between methylene chloride and 1.0M hydrochloric acid. The organic layer was dried (anhydrous magnesium sulfate), filtered. The residue was purified by flash chromatography (120 g of silica gel, eluting with a gradient of ethyl acetate in hexanes) to give methyl 4-(cyano-dimethylmethyl)-2-ethoxy- benzoate (1.09 g, 55%). LR-MS: 248.19 [(M+H)@]

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.

Reference:
Patent; F.HOFFMANN-LA ROCHE AG; WO2005/110996; (2005); A1;,
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Application of 107622-80-0, 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. 107622-80-0, name is (4-Phenoxyphenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: The appropriate pyrazole (1.0 equiv) was treated with phosgene(20% in toluene) at 0 C. The reaction mixture was stirred at room temperature for 1 h.The solvent was removed under reduced pressure and the crude carbamoyl chloride was redissolved in anhydrous CH2Cl2 (0.5 M). The appropriate amine (1.0 equiv) and Et3N (1.2 equiv) were dissolved in CH2Cl2 and cooled to 0 C. The crude carbamoyl chloride was added dropwise and the reaction mixture was stirred at room temperature for 16 h.The mixture was diluted with EtOAc, washed with saturated aqueous NaCl, and dried over Na2SO4. Evaporation under reduced pressure yielded the crude coupling product that was purified by flash chromatography (SiO2).

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

Reference:
Article; Otrubova, Katerina; Srinivasan, Venkat; Boger, Dale L.; Bioorganic and Medicinal Chemistry Letters; vol. 24; 16; (2014); p. 3807 – 3813;,
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Application of 39538-68-6, 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. 39538-68-6, name is 2-Methoxy-4-methylaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Malonyl diamide derivatives were prepared as described earlier.49 Briefly: To a magnetically stirred ice bath-cooled solution of the selected amine (14 mmol), and triethylamine (14 mmol, 1.4 g) in dioxane (20 ml), malonyl dichloride (1.0 g, 7.0 mmol) solution in dioxane (20 ml) was added dropwise over 15 min. The reaction mixture was stirred at 0 C for one hour. Subsequently, HCl (2 N, 50 ml) was added to the reaction suspension and stirred for 30 minutes. Finally, the mixture was filtered to afford the products as whitish to gray solids that were further washed by stirring in water (50 mL) for 30 min (Scheme 1).

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, 2-Methoxy-4-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Habash, Maha; Taha, Mutasem O.; Bioorganic and Medicinal Chemistry; vol. 19; 16; (2011); p. 4746 – 4771;,
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These common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, 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. Recommanded Product: 7252-83-7

(1) Synthesis of 1-(2,2-Dimethoxyethylsulfanyl)-4-fluorobenzene In a nitrogen stream, 4-fluorobenzenethiol (2.5 ml, 23.4 mmol) and 2-bromo-1,1-dimethoxyethane (3.0 ml, 25.7 mmol) were added to a sodium methoxide methanol solution (0.5 M, 74.9 ml, 37.4 mmol) under cooling with ice and the reaction mixture was stirred at the same temperature for 10 minutes, and then heated and refluxed for five hours. The reaction mixture was concentrated under reduced pressure, and added with cold water. The mixture was extracted with ether. The organic layer was washed with a saturated sodium chloride aqueous solution, and then dried with sodium sulfate. After filtration, the solvent was distilled under reduced pressure, and the obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate: n-hexane (1:20)] to obtain the title compound (4.52 g, 89%). 1H-NMR (CDCl3) delta: 3.05 (2H, d, J=5.4 Hz), 3.35 (6H, s), 4.49 (1H, t, J=5.4 Hz), 6.85 (2H, t, J=9.0 Hz), 7.31 (2H, dd, J=8.7, 5.1 Hz)

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

Reference:
Patent; CHUGAI SEIYAKU KABUSHIKI KAISHA; EP1803721; (2007); A1;,
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