Synthesis
To a 50 mL pressure-resistant reaction tube (equipped with a PTFE high-pressure valve) equipped with a magnetic stirrer, copper(II) trifluoromethanesulfonate (Cu(OTf)2, 0.05 mmol), octanoic acid (0.5 mmol), N,N-dimethylformamide (2.0 mmol), di-tert-butyl peroxide (DTBP, 1 mmol), and 1,2-dichloroethane (DCE, 1 mL) were added in sequence. 1 mL). The reaction mixture was stirred in an oil bath at 130 °C for 12 h and subsequently cooled to room temperature. The reaction solution was diluted with ethyl acetate and filtered through a diatomaceous earth pad. The filtrate was washed sequentially with saturated aqueous sodium bicarbonate solution (5 mL) and saturated aqueous sodium chloride solution (5 mL x 2). The organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to remove the solvent. The residue was purified by preparative thin layer chromatography (TLC) on silica gel to afford the target product N,N-dimethyloctanamide.
References
[1] Chinese Chemical Letters, 2015, vol. 26, # 1, p. 11 - 14
