反应详情

Sodium hydride (60% dispersion in oil, 2.45 g) was added to ethanol (100 ml), to which was added 3-carboethoxy-2-piperidone (10.0 g). The reaction mixture was stirred for 15 minutes, to which was added 2-nitrobenzyl bromide (13.2 g) at room temperature. The reaction mixture was stirred at 60° C. for 3 hours. Water was added to the reaction mixture, which was concentrated. The residue was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried and concentrated. The obtained crude crystals were recrystallized from ethyl acetate-hexane to give the entitled compound (14.6 g).

1. stirringThe reaction mixture was stirred at 60° C. for 3 hours
2. concentrationwas concentrated
3. additionThe residue was diluted with water
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materiala saturated aqueous sodium chloride solution, then dried
7. concentrationconcentrated
8. customThe obtained crude crystals
9. customwere recrystallized from ethyl acetate-hexane