Tag: M.W=200-300

Reference of 886762-08-9, 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 886762-08-9 as follows.

General procedure: To a stirred solution of 5-bromo-2-(trifluoromethoxy)aniline (540 mg, 2.11 mmol) in pyridine was added pyridine-2-sulfonylchloride (410 mg, 2.31 mmol and the mixture was heated to 45C for 4 h. After quenchingwith water the mixture was extracted with CH2C12, dried over MgSO4 and evaporated togive a solid (769 mg) that was used without further purification. To a mixture of the aforementioned crude solid and (chloromethoxy)ethane (329 mg, 3.49 mmol) in DMF at room temperature was added a 60% w/w dispersion of Nail in mineral oil (140 mg, 3.49 mol) and the mixture was stirred for 1 h. After quenching with water the mixture was extracted with CH2CI2, dried with MgSO4 and evaporated to give a solid which waspurified by column chromatography eluting with hexanes/EtOAc 3:1. The title compound was isolated as a colourless oil (857 mg, 89%, 2 steps).?H NMR [400 MHz, CDCI3I 6 8.75 (ddd, J =4.8, 1.6, 1.0 Hz, 1H), 7.90-7.82 (m, 2 H), 7.54-7.46 (m, 3 H), 7.10 (dddd, J = 8.9, 1.9,1.8, 1.8 Hz, 1 H), 5.21 (br s, 2 H), 3.79 (q, J = 7.0 Hz, 2 Fl), 1.20 (t, J = 7.0 Hz, 3 H). LRMS (APCI?) calcd for C13H10BrF3N2O3S 409 (M-EtO), found 409.

According to the analysis of related databases, 886762-08-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PETER MACCALLUM CANCER INSTITUTE; SPICER, Julie Ann; DENNY, William Alexander; MILLER, Christian Karl; O’CONNOR, Patrick David; HUTTUNEN, Kristiina; TRAPANI, Joseph A.; HILL, Geoff; ALEXANDER, Kylie; WO2014/28968; (2014); 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 886762-08-9 as follows. HPLC of Formula: C7H5BrF3NO

Under nitrogen atmosphere, 2.2 mL of anhydrous triethylamine was added dropwise to a solution of 2 g (15.4 mmol) of 1,1-cyclopropanedicarboxylic acid in dichloromethane, and the mixture was stirred for 30 min in an ice bath and then 1.2 mL SOCl2 in dichloromethane,After the addition was complete, the mixture was stirred for 2h, and then 3.5g (13.9mmol) of 5-bromo-2-trifluoromethoxyaniline in dichloromethane was added dropwise to the reaction mixture. After the addition was completed, stirring was continued for 2h. The reaction solution was then adjusted to pH 10 with 2 mol / L NaOH solution, evaporated to dryness under reduced pressure, sonicated with appropriate amount of water, extracted once with ethyl acetate, the aqueous layer was retained,The aqueous layer was further adjusted to pH 2 with 2 mol / L HCl and extracted three times with ethyl acetate.The organic solvent was removed under reduced pressure to give 1 – ({[5-bromo-2- (trifluoromethoxy) phenyl] amino} carbonyl) cyclopropanecarboxylic acid, About 0.8g, yield 35%;

According to the analysis of related databases, 886762-08-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Xi’an Jiaotong University; Zhang Jie; Lu Wen; Su Ping; Wang Jinfeng; Pan Xiaoyan; He Langchong; Wang Sicen; He Huaizhen; (14 pag.)CN105924403; (2016); A;,
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Related Products of 701-07-5, 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 701-07-5 as follows.

To a suspended solution of Mg chips (10.07 g, 0.414 mol) in anhydrous ether (150 mL) at 22C under argon was added ca. 0.15 mL of 1,2-dibromoethane. Then 43.7 g (0.200 mol) of 2-(isopropoxy)bromobenzene in 200 mL of ether was added dropwise. After 50% of the aryl halide was added, the reaction began to reflux vigorously. The flask was cooled in an ice bath. After the refluxing had subsided somewhat, the ice bath was removed and the remaining aryl halide was added over a 1.5 h period. The resultant Grignard reagent was cooled in a dry ice/ether bath for 2 h and then treated with 34.0 mL (0.221 mol) of 98% 1-carbethoxy-4-piperidone. Upon complete addition of ketone, the reaction mixture was allowed to warm to 22C and stirred for 2 h. The reaction was then quenched with cold aqueous ammonium chloride which resulted in an emulsion. Addition of 1M aqueous HCI solution separated the two layers. The aqueous phase was extracted with additional ether and the combined organic solution was washed with 10% aqueous sodium bisulfite, 1.0 M HCI, saturated NaHCO3, and dried (K2CO3). Filtration and concentration yielded 56.36 g of 1-carbethoxy-4-[2-(1-methylethoxy)phenyl]-4-piperidinol as a yellow viscous oil which was carried on without further purification The structure of this oil was supported by 1H NMR.

According to the analysis of related databases, 701-07-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ORTHO PHARMACEUTICAL CORPORATION; EP736009; (2002); B1;,
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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. 2674-34-2, name is 1,4-Dibromo-2,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Product Details of 2674-34-2

A flame dried RBF was charged with l,4-dibromo-2,5-dimethoxybenzene (1) (10.3 g, 39.6 mmol, 1.0 equiv.), phenylboronic acid (9.92 g, 81.4 mmol, 2.05 equiv.), potassium carbonate (19.2 g, 139 mmol, 3.5 equiv.), toluene (80 mL), deionized water (40 mL), and a stir bar. Pd(PPh3)4 (457 mg, 0.395 mmol, 1 mol%) was added last to the flask before the reaction mixture was lowered into a bath that was preheated to 90 C and stirred for l2h with a condenser. Upon completion, the reaction was diluted with water, extracted 3 times with DCM, dried on MgS04, and concentrated via rotary evaporation. The solid was then recrystallized in EtOH to provide 9.01 g (31.1 mmol, 78% yield) of white needles. NMR (500 MHz, CDCb): d 7.61-7.59 (m, 4H), 7.46-7.43 (m, 4H), 7.38-7.34 (m, 2H), 6.99 (s, 2H), 3.80 (s, 6H). 13C NMR (125 MHz, CDCb): d 150.6, 138.3, 130.4, 129.4, 128.1, 127.1, 114.8, 56.4. HRMS (TOF-EI, m/z) calcd. for C20H18O2 [M]+: 290.1307; found: 290.1300.

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; LEHIGH UNIVERSITY; CHEN, Mark; WEHRMANN, Caleb; CHARLTON, Ryan; (58 pag.)WO2019/226678; (2019); A2;,
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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. 262587-05-3, name is 1-Bromo-3-(difluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

A mixture of commercially available 1-boc piperazine (500.1 mg, 2.685 mmol) and commercially available 3-difluoromethoxybromobenzene (598.8 mg, 2.685 mmol) in toluene (20 ml) is placed in a 50 ml three-necked round-bottomed flask made inert with argon, and then the ligand (R)-(+)-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (56.850 mg, 91.2 mumol) and palladium(II)acetate (20.4 mg, 91.2 mumol) are added. The reaction mixture is stirred and brought to reflux for 16 hours. After returning to 20 C., the reaction mixture is diluted with water (20 ml) and then extracted with ethyl acetate (2*30 ml). The organic extracts are combined, dried over magnesium sulfate, filtered and evaporated under reduced pressure. The compound obtained is purified by chromatography on silica gel (AIT cartridge, Ref. FC-25 Si-BP-SUP, 20-40 mum, eluent dichloromethane, flow rate 20 ml/min). The fractions containing the expected compound are combined and then evaporated under reduced pressure. The expected tert-butyl 4-(3-difluoromethoxyphenyl)piperazin-1-ylcarboxylate is isolated (253 mg), the characteristics of which are as follows: LC/MS analysis: tr=4.18 min, M+H+ 329.31

According to the analysis of related databases, 262587-05-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharma S.A.; US2005/14765; (2005); A1;,
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Related Products of 54314-84-0, 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. 54314-84-0, name is ((3-Bromopropoxy)methyl)benzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

N- (benzyloxycarbonyl) acetamide potassium salt(76 mg, 0.33 mmol) and 18-crown-6 (79 mg, 0.30 mmol)Was dissolved in dimethylformamide (1.7 mL).Benzyl 3-bromopropyl ether (50 mL, 0.30 mmol) was added, followed by stirring at room temperature for 20 hours.The reaction was terminated by adding saturated aqueous ammonium chloride solution (about 3 mL)The reaction mixture was extracted with ethyl acetate.After washing the organic layer with water and saturated brine,And dried over anhydrous magnesium sulfate.Purification by flash silica gel chromatography (20percent ethyl acetate / n-hexane)A colorless oil of N- (3- (benzyloxy) propyl) -N- (benzyloxycarbonyl) acetamide (91 mg, 89percent) was obtained.

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, ((3-Bromopropoxy)methyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; School corporation Meijo University; Mori, Yuji; Sakai, Takeo; Fukuda, Ayumi; Kasai, Satomi; (28 pag.)JP2018/95576; (2018); A;,
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Adding a certain compound to certain chemical reactions, such as: 5467-58-3, name is 1-Bromo-4-methoxynaphthalene, 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 5467-58-3, Product Details of 5467-58-3

[00395] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (21 mg; 0.026 mmol) and triethylamine (0.34 ml; 2.44 mmol) in dioxane (2.5 ml; dried over 4 A sieves) was sealed and stirred at 80 C. overnight (18 h). After cooling to room temperature, HB(pin) (0.19 ml; 1.31 mmol) was added followed by 1-bromo-4-methoxynaphthalene (207 mg; 0.873 mmol) in dioxane (2.5 ml; dried over 4 A sieves) the reaction mixture was stirred at 80 C. GC analysis after 2 days showed the desired borate compound at 14.7 minutes.

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-4-methoxynaphthalene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
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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 74137-36-3 as follows. Safety of 1,3-Dibromo-5-methoxybenzene

Tris (dibenzylideneacetone) [DIPALLADIUM (0)] (6.53g, 7. [15MMOL)] was added in one portion to a stirred solution of the bromide of Preparation 1 (38. 0g, [143MMOL),] 1,1′-bis (diphenylphosphino) ferrocene (9.3g, 16. [8MMOL)] and zinc cyanide (20. 0g, [172MOL)] in N,N-dimethylformamide (300ml) at room temperature under nitrogen. The reaction was heated at [100¡ãC] for 14 hours and cooled to room temperature. Water (1500ml) was added and the mixture was extracted with ethyl acetate [(3X500ML).] The combined organics were filtered and the filtrate was washed with water (500ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure. The resulting solid was triturated with toluene (1000ml) to provide the title compound (18. 0g) as a tan solid.

According to the analysis of related databases, 74137-36-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfizer Limited; Pfizer Inc.; WO2004/31156; (2004); A1;,
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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. 101-55-3, name is 1-Bromo-4-phenoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-phenoxybenzene

General procedure: The chemical synthesis was started with chlorosulfonylationof the substituted benzenes (S1) individually in dry chloroformby dropwise addition of chlorosulfonic acid over a period of45-60 mins at 0-5 C. After completion of chlorosulfonic acid addition,the reaction mixture was stirred for additional 45 min atroom temperature and the mixture was poured over crushed ice.The mixture was extracted thrice with 50 ml chloroform whichwas dried overnight in presence of anhydrous sodium sulfate. Afterevaporation of the solvent chloroform, substituted benzenesulfonylchlorides (I1) were obtained individually in solid formswhich were used for next step without any purification.

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:
Article; Adhikari, Nilanjan; Halder, Amit K.; Mallick, Sumana; Saha, Achintya; Saha, Kishna D.; Jha, Tarun; Bioorganic and Medicinal Chemistry; vol. 24; 18; (2016); p. 4291 – 4309;,
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Reference of 16618-68-1, These common heterocyclic compound, 16618-68-1, name is 3-Bromo-5-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.

In 50 ml by adding three-necked bottle 1.01g3-methoxy-5-bromoaniline(5mmol), 1.40g (5.5mmol) connecting boric acid frequency ester, 1.47g (15mmol) and potassium acetate PdCl2(dppf) catalyst (150 mg), vacuum pumping and nitrogen injection 6 times, the state of the protection of nitrogen by adding DMSO (25 ml), 80 C reaction 18h, in a water cooling retrodisplacement, precipitate after filtering, washing, drying to obtain the crude column chromatography separation (petroleum ether: ethyl acetate = 1:5) shall be 1.03g yellow powdery solid, yield 82.4%.The 0.99g the above-mentioned preparation of the compound (4mmol) by adding 100 ml round-bottom flask, add 30 ml of methanol is dissolved, add 0.56gNH4Cl (10mmol), constant voltage dropping funnel for slowly dripping 2.56gNaIO4(12mmol) of 7 ml aqueous solution, stirring the mixture at room temperature for reaction 18h, TLC detection, filtering to remove the inorganic salt, methanol filters after evaporation to dryness, drying to obtain the crude product purification column chromatography (petroleum ether: ethyl acetate = 1:5) shall be near white powdery solid 0.53g, yield 79.1%.

The synthetic route of 16618-68-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ocean University of China; Jiang, Tao; Yin, ruijuan; Zhang, Li Juan; (38 pag.)CN103497211; (2016); B;,
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