反应详情

2-(3-bromopropoxy-7-hydroxymethyl-4-isopropyl-2,4,6-cycloheptatrien-1-one (280 mg, 0.89 mmol), N-phenethylamine (0.15 ml, 1.03 mmol), triethylamine (0.15 ml, 1.08 mmol) were dissolved in chloroform (5 ml), and the solution was heated and refluxed for 5 hours. The solution was diluted with dichloromethane, washed with water and dried over sodium sulfate. After solvent was distilled off under reduced pressure, the residue was purified by silica gel column chromatography [eluent:chloroform/methanol (10:1)] to give 242 mg of 7-hydroxymethyl-4-isopropyl-2-[3-(N-methyl-N-phenethylamino)propoxy]-2,4,6-cycloheptatrien-1-one as a yellowish brown oil (yield: 74%).

1. temperaturethe solution was heated
2. temperaturerefluxed for 5 hours
3. washwashed with water
4. dry with materialdried over sodium sulfate
5. distillationAfter solvent was distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography [eluent:chloroform/methanol (10:1)]