Electric Literature of 57946-63-1, 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 57946-63-1 as follows.
EXAMPLE 6 4-(2-Bromo-4-trifluoromethyl-phenylcarbamoyl)-piperidine-1-carboxylic acid tert-butyl ester Piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (4.90 g, 21.00 mmol) was dissolved in dry methylene chloride (30 mL) and dry pyridine (4.30 mL). To the reaction mixture was then added thionyl chloride (3.00 g, 25.20 mmol) under nitrogen atmosphere and the reaction mixture was stirred at room temperature for 30 minutes. To the reaction mixture was then added successively, under nitrogen atmosphere, 2-bromo-4-trifluoromethyl-phenylamine (5.60 g, 23.50 mmol), dry triethylamine (7.43 g, 73.5 mmol), dry methylene chloride (38 mL), 4-(dimethylamino)pyridine (0.26 g, 2.18 mmol) and the reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was then partitioned with aqueous 2N HCl and tert-butyl methyl ether. The organic layer was washed with aqueous 2N HCl, aqueous NaHCO3, brine, dried with Na2SO4, filtered and the solvent evaporated in vacuo to yield a crude oil. The crude oil was purified via flash chromatography (30percent ethyl acetate/hexanes) to yield the title compound as an oil. 1H NMR (300 MHz, CDCl3) delta 8.5 (1H, d, J=9 Hz), 7.6 (1H, bs) 7.5 (1H, d, J=7.0 Hz), 7.3 (1H, d, J=8 Hz), 4.18 (2H, m), 2.8 (2H, m), 1.9 (2H, d), 1.8 (2H, m), 1.47 (9H, s) MS (ES+) m/z 475.0 (MNa)+
According to the analysis of related databases, 57946-63-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Battista, Kathleen A.; Bignan, Gilles C.; Connolly, Peter J.; Liu, Jessica J.; Middleton, Steven A.; Orsini, Michael J.; US2007/112016; (2007); A1;,
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