반응 #415349

ord-bae7d0942c714db0bf3630cafccbeb6d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 3 hours
  2. 2
    농축the reaction mixture was concentrated
  3. 3
    workup.ADDITION20ml of methanol and 2ml of sulfuric acid were added to the residue
  4. 4
    온도the mixture was refluxed for one hour
  5. 5
    농축After the methanol was concentrated
  6. 6
    workup.ADDITIONthe water was added to the residue
  7. 7
    추출extracted with ether
  8. 8
    세척The extract was washed over magnesium sulfate
  9. 9
    workup.DISTILLATIONthe ether was distilled off
  10. 10
    workup.DISTILLATIONThe residue was distilled under reduced pressure
  11. 11
    기타to give the object compound

실험 절차

In a mixture of 12ml of hydroiodic acid, 90ml of acetic acid and 1g of phosphorus 10g of 2-(4-methoxyphenyl)propionic acid was refluxed for 3 hours and the reaction mixture was concentrated. 20ml of methanol and 2ml of sulfuric acid were added to the residue and the mixture was refluxed for one hour. After the methanol was concentrated, the water was added to the residue and extracted with ether. The extract was washed over magnesium sulfate and the ether was distilled off. The residue was distilled under reduced pressure to give the object compound having b.p. 150° - 153° C/6mm Hg in a yield of 6.7g (67%)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04016193uspto-grants-1977_04