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;,
Ether – Wikipedia,
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