Toluene → HCID 86695295, compound

Participants

Reaction Conditions

Reaction Steps

28.20 g (0.125 mol) of 1-(2,4-difluorobenzyl)-4-piperidone crude product was added to a reaction bottle, to which 200 mL of toluene was added. The reaction was heated and stirred at 80° C. in an oil bath, and to the reaction 29.60 g (0.135 mol) of trimethylsulfoxide iodide and 0.60 g (0.0018 mol) of tetrabutylammonium hydrogen sulfate were added in sequence and then 11.40 g (0.285 mol) of sodium hydroxide dissolved in 60 mL of aqueous solution was added dropwise under stirring. After the addition, the reaction was continuously stirred at bath temperature of 80° C. overnight. On the next day, the reaction was cooled, washed with water twice, extracted with a small amount of toluene, combined and dried, and the solvent was recovered to obtain light yellow liquid 22.00 g (73.6%), i.e., a crude target product, 1H-NMR (CDCl3, ppm) δ: 7.361 (1H, m), 6.76-6.89 (2H, m), 3.597 (2H, d, J=1.12 Hz), 2.651 (2H, s), 2.601 (4H, m), 1.829 (2H, m), 1.545 (2H, m).

Provenance & Evidence