반응 #571227

ord-eccc3a4ff480432f8bdb32903b64b671

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the bottle was sealed
  2. 2
    추출extracted with EtOAc
  3. 3
    세척The combined organic extracts were washed successively with saturated NaHCO3, H2O (twice) and brine
  4. 4
    건조before being dried over Na2SO4
  5. 5
    기타evaporated to dryness
  6. 6
    기타Crystals formed
  7. 7
    workup.WAITafter standing overnight
  8. 8
    여과they were filtered
  9. 9
    세척washed with cold hexane
  10. 10
    기타dried

실험 절차

A solution of H2SO4 (5 ml) in dioxane (80 ml) was added to 4-hydroxyphenylacetic acid (20 gm, 0.13 mol) in a pressure bottle. Isobutylene (250 ml) was added and the bottle was sealed and the mixture was stirred for 24 hr. The reaction mixture was poured into saturated NaHCO3 solution and extracted with EtOAc. The combined organic extracts were washed successively with saturated NaHCO3, H2O (twice) and brine before being dried over Na2SO4 and evaporated to dryness. Crystals formed after standing overnight and they were filtered, washed with cold hexane and dried to give 20.99 gm of the title compound. M.pt. 95°-96° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05229381uspto-grants-1993_07