반응 #2474134

ord-4ead1654c0d74347bd8974373ea00ae3

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  2. 2
    workup.DISTILLATIONdistilled water
  3. 3
    workup.ADDITIONwas added
  4. 4
    추출and the mixture extracted with ethyl acetate
  5. 5
    건조The organic phase was dried with anhydrous sodium sulfate
  6. 6
    기타the product purified by silica gel column chromatography (chloroform/methanol=20/1)

실험 절차

2-(4-hydroxyphenyl)-3-methyl-1(2H)-isoquinolinone (30 mg, 0.12 mmol), 1-(3-bromopropyl)piperidine hydrobromide (51 mg, 0.18 mmol) and potassium carbonate (49 mg, 0.36 mmol) were mixed in dimethylformamide (3 mL) and stirred at 80° C. for 3 hours. The solvent was distilled off under reduced pressure, distilled water was added. and the mixture extracted with ethyl acetate. The organic phase was dried with anhydrous sodium sulfate, and the product purified by silica gel column chromatography (chloroform/methanol=20/1) to obtain the title compound (18 mg, 40%) as a colorless solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08268842B2uspto-grants-2012_09