反应 #5305

ord-17aed5b9702b46f69ddfc58fdccf4fd4

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The resulting suspension was refluxed for 27 h
  2. 2
    萃取The mixture was extracted with ER (2×200 ml)
  3. 3
    萃取the dried extract
  4. 4
    其他was evaporated
  5. 5
    其他to leave an orange oil
  6. 6
    其他The oil was purified on a column of silica (800 ml) [A]
  7. 7
    其他to give a yellow oil which
  8. 8
    workup.DISTILLATIONon distillation

实验过程

NaH (46% dispersion in oil; 6.5 g) was added portionwise to a solution of 4-phenyl-1-butanol (15.0 g) and 1,6-dibromohexane (48.8 g) in THF (200 ml) under nitrogen. The resulting suspension was refluxed for 27 h and treated with H2O (80 ml). The mixture was extracted with ER (2×200 ml) and the dried extract was evaporated to leave an orange oil. The oil was purified on a column of silica (800 ml) [A] to give a yellow oil which on distillation gave the title compound as a colourless oil (15.0 g) b.p. 90-95/0.1 mmHg.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05243076uspto-grants-1993_09