반응 #54733

ord-54cc47a78449481494b15c343d1d17db

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the mixture was reacted at room temperature for 2 hours
  2. 2
    기타the crystals produced
  3. 3
    기타were removed by filtration
  4. 4
    workup.DISTILLATIONThe filtrate was freed of solvent by distillation
  5. 5
    기타to leave a residue
  6. 6
    추출The resulting mixture was extracted with ether
  7. 7
    추출The ether extract
  8. 8
    workup.DISTILLATIONfreed of ether by distillation
  9. 9
    기타The oily residue thus obtained
  10. 10
    workup.DISTILLATIONwas distilled in vacuo

실험 절차

To a solution of 2.2 g of 2-pyridinemethanol in 20 ml of tetrahydrofuran were added 3 g of 2-(4-isobutylphenyl)propionic acid chloride and subsequently 2.7 g of triethylamine, and the mixture was reacted at room temperature for 2 hours. After the reaction was complete, the crystals produced were removed by filtration. The filtrate was freed of solvent by distillation to leave a residue, to which was added water. The resulting mixture was extracted with ether. The ether extract was dehydrated and freed of ether by distillation. The oily residue thus obtained was distilled in vacuo to give 3.5 g of 2-(4-isobutylphenyl)propionic acid-2-pyridylmethyl ester as a pale yellow oil, boiling at 138°-140° C./0.15 mmHg. Mass spectrum: parent ion 297 m/e.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04150137uspto-grants-1979_04