HRID322606

反应详情

EQUATION

反应方程式

HRID 322606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A 250 ml flask is charged with 15 g (34.5 mmol, 2.2 eq) of bromide (2) and acetone (100 ml) under an argon atmosphere. To this solution is added 3,5-dihydroxybenzyl alcohol (2.2 g, 15.7 mmol), 0.82 g (31. mmol, 0.2 eq) 18-C-6 and 4.77 g (34-5 mmol, 2.2 eq) of K2CO3 and the mixture is stirred for 48 hours whereupon a yellow suspension is formed. To the mixture is added methylene chloride (200 ml) and water (200 ml). The organic phase is separated, dried over MgSO4 and evaporated to dryness. A dark brown oil is obtained which is dissolved in toluene (40 ml) and hexane (20 ml). Upon cooling, a white powder forms which is collected by filtration to give 10.92 g (81.9% of (3A).

WORKUP

后处理

  1. customis formed
  2. customThe organic phase is separated
  3. dry with materialdried over MgSO4
  4. customevaporated to dryness
  5. customA dark brown oil is obtained which
  6. temperatureUpon cooling
  7. filtrationa white powder forms which is collected by filtration