反应详情

17.6 g (0.10 mol) of (indan-2-yl)acetic acid was dissolved in 150 ml of toluene, to which were added 15.3 ml (0.11 mol) of triethylamine and 33.0 g (0.12 mol) of diphenylphosphorylazide, and stirred at room temperature for 30 minutes. The mixture was added with 16.6 g (0.15 mol) of benzyl alcohol and refluxed for 18 hours. After cooling, the solvent was distilled under reduced pressure, and the residue was added with 500 ml of ethyl acetate, washed with 1N sodium hydroxide, and condensed. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:3), and the crystals collected were recrystallized from a solvent mixture of ethyl acetate and hexane to obtain 24.3 g of 2-(benzyloxycarbonylaminomethyl)indan as colorless needles. Yield: 86%

1. temperaturerefluxed for 18 hours
2. temperatureAfter cooling
3. distillationthe solvent was distilled under reduced pressure
4. additionthe residue was added with 500 ml of ethyl acetate
5. washwashed with 1N sodium hydroxide, and condensed
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:3)
7. customthe crystals collected
8. customwere recrystallized from a solvent mixture of ethyl acetate and hexane