HRID5212

反应详情

EQUATION

反应方程式

HRID 5212 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; 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.

WORKUP

后处理

  1. temperatureThe suspension was refluxed for 20 h
  2. extractionThe resulting emulsion was extracted with ER (2×50 ml)
  3. extractionthe dried extract
  4. customwas evaporated
  5. customto leave a yellow oil
  6. customThe oil was purified on a column of silica (Merck 9385, 600 ml) [A]