反应 #415349

ord-bae7d0942c714db0bf3630cafccbeb6d

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 3 hours
  2. 2
    浓缩the reaction mixture was concentrated
  3. 3
    workup.ADDITION20ml of methanol and 2ml of sulfuric acid were added to the residue
  4. 4
    温度the mixture was refluxed for one hour
  5. 5
    浓缩After the methanol was concentrated
  6. 6
    workup.ADDITIONthe water was added to the residue
  7. 7
    萃取extracted with ether
  8. 8
    洗涤The 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
    其他to give the object compound

实验过程

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%)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04016193uspto-grants-1977_04