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 25625-57-4 as follows. Quality Control of 2-Bromo-N-(3-(trifluoromethyl)phenyl)acetamide
Example 5: 2-[3-(4-Bromophenyl)-2-oxo-7-oxa-1 ,4-diazaspiro[4.5]dec-3-en-1 -yl]-N-[3- (trifluoromethyl)phenyl]acetamide; 3-(4-Bromophenyl)-7-oxa-1 ,4-diazaspiro[4.5]dec-3-en-2-one (D19) (100mg, 0.32mmol) in DMF (4ml) was cooled to ice bath temp and treated with sodium hydride (14.23 mg, 0.356 mmol) under an atmosphere of argon. The mixture was stirred for 30 minutes then 2- bromo-N-[3-(trifluoromethyl)phenyl]acetamide (D16) (100 mg, 0.356 mmol) in DMF (2ml) was added over 1.5 hour by syringe pump. The mixture was then allowed to warm to room temp overnight. The mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with brine and dried using sodium sulphate and the solvent was removed. The residue was chromatographed on a silica column eluted with a gradient of 0-5% methanol in DCM. A mixture was obtained which was purified by low pH MDAP to give the title compound (81 mg).1H NMR (d6DMSO) delta: 1.65-1.80 (2H, m), 2.06-2.28 (2H, m), 3.5 (1 H, m), 3.65 (1 H, m), 3.8-3.95 (2H, m), 4.5 (2H, m), 7.42 (1 H, m), 7.61 (1 H, m), 7.77 (3H, m) 8.08 (1 H, m), 8.32 (2H, s), 10.6 (1 H, s). 19F NMR (DMSO) delta: -61.4 (s), Mass Spectrum (Electrospray LC/MS): Found 510 (MH+). Ret. time 3.33 min.
According to the analysis of related databases, 25625-57-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; GLAXO GROUP LIMITED; UNIVERSITY OF NOTTINGHAM; WO2008/92877; (2008); A2;,
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