반응 #5308

ord-ac03c135aa2e493cb63eaf76ba6c32fa

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The suspension was refluxed for 20 h
  2. 2
    추출The resulting emulsion was extracted with ER (2×50 ml)
  3. 3
    추출the dried extract
  4. 4
    기타was evaporated
  5. 5
    기타to leave a yellow oil
  6. 6
    기타The oil was purified on a column of silica (Merck 9385, 600 ml) [A]

실험 절차

NaH (46% dispersion in oil; 1.36 g) was added portionwise to a solution of 2-methoxybenzenebutanol (5.0 g) and 1,6-dibromohexane (13.8 g) in THF (50 ml). The suspension was refluxed for 20 h and was treated cautiously with H2O (20 ml). The resulting emulsion was extracted with ER (2×50 ml) and the dried extract was evaporated to leave a yellow oil. The oil was purified on a column of silica (Merck 9385, 600 ml) [A] to give the title compound as a colourless oil (5.6 g). T.l.c. [B] Rf 0.2.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05243076uspto-grants-1993_09