반응 #466274

ord-bae778c2af4040f99eed4339b68dca3e

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was refluxed for 24 hours
  2. 2
    기타The solid was removed by filtration
  3. 3
    기타the solvent was evaporated
  4. 4
    기타The residue was partitioned between EtOAc and H2O
  5. 5
    건조dried over Na2SO4
  6. 6
    기타The solvent was evaporated

실험 절차

To a suspension of 4-oxopiperidine hydrochloride monohydrate (10.0 g, 65.1 mmol) and methyl 3-bromopropanoate (7.8 ml, 71.6 mmol) in acetone (100 ml) was added K2CO3 (9.9 g, 71.6 mmol) and Et3N (9.1 ml, 65.3 mmol). The mixture was refluxed for 24 hours. The solid was removed by filtration and the solvent was evaporated. The residue was partitioned between EtOAc and H2O. The organic extracts were combined and dried over Na2SO4. The solvent was evaporated to give the title compound (15.0 g, 27.0 mmol, 42%) as an oil. 1H NMR (300 MHz, CDCI) δ 3.70 (s, 3H), 2.75-2.85 (mult, 6H), 2.52-2.57 (mult, 2H), 2.42-2.46 (mult, 4H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06297260B1uspto-grants-2001_10