반응 #2561

ord-6f48f4894ab44bc5ac2137804fdccac1

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at room temperature
  2. 2
    기타the resulting reaction solution
  3. 3
    추출was extracted with chloroform
  4. 4
    세척washed with saturated brine
  5. 5
    건조The resulting organic layer was dried on anhydrous magnesium sulfate
  6. 6
    기타the solvent was removed by evaporation
  7. 7
    workup.ADDITIONthe resulting residue was mixed with 5 ml of chloroform
  8. 8
    기타to remove insoluble materials
  9. 9
    여과by filtration

실험 절차

N-(2-Methoxyphenyl)-N-(1,3-dioxolan-2-yl)methyl-4-phthalimidomethylbenzamide (450 mg, 0.953 mmol) was dissolved in THF (6 ml) to which was subsequently added 10% hydrochloric acid (4 ml) at room temperature. After 2 hours of stirring at 60° C., the resulting reaction solution was extracted with chloroform and washed with saturated brine. The resulting organic layer was dried on anhydrous magnesium sulfate, the solvent was removed by evaporation and then the resulting residue was mixed with 5 ml of chloroform to remove insoluble materials by filtration, thereby obtaining 300 mg (73.5%) of the title compound in the form of yellow oil which was used in the subsequent reaction without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728835uspto-grants-1998_03