HRID5209

反应详情

EQUATION

反应方程式

HRID 5209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.

WORKUP

后处理

  1. temperatureThe resulting suspension was refluxed for 27 h
  2. extractionThe mixture was extracted with ER (2×200 ml)
  3. extractionthe dried extract
  4. customwas evaporated
  5. customto leave an orange oil
  6. customThe oil was purified on a column of silica (800 ml) [A]
  7. customto give a yellow oil which
  8. distillationon distillation