반응 #347765

ord-77f0e122c74e443c94935fabe604c557

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ether
  2. 2
    세척the organic phase was washed
  3. 3
    건조dried over sodium sulfate
  4. 4
    기타evaporated under reduced pressure
  5. 5
    기타Two recrystallizations of the residue from methanol

실험 절차

27.5 g (0.2 mol) of anhydrous aluminum chloride were added by spatula to 250.0 g (2.65 mol) of phenol plus 414.5 g (2.27 mol) of 2,5-dichloro-2,5-dimethylhexane in 500 ml of petroleum ether at room temperature while stirring. After 48 hours, the reaction mixture was poured into ice-water and extracted with ether, and the organic phase was washed to neutrality with water, dried over sodium sulfate and evaporated under reduced pressure. Two recrystallizations of the residue from methanol yielded 148.7 g of the title compound of melting point 219°-220° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05527945uspto-grants-1996_06