HRID1085631

反应详情

EQUATION

反应方程式

HRID 1085631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Propyl bromide (29.2 mL, 0.32 mol) was added to a solution of 5-iodovanillin (50.0 g, 0.18 mol) in DMF (200 mL) containing potassium carbonate (48 g, 0.35 mol) at 80° C. The mixture was stirred at 80° C. for 1-1.5 hours or until TLC (SiO2, 4:1 [v/v] hexane-ethyl acetate) showed the reaction to be complete. The mixture was cooled and the solvent was decanted into ice-water (1 L). The product was extracted with ether and the ethereal layer was washed with water, dried over sodium sulfate, and evaporated in vacuo to an oil, which was used without further purification. Anal. calc. for C11H15IO3 : C, 41.27; H, 4.09. Found: C, 41.59; H, 4.15.

WORKUP

后处理

  1. customthe reaction
  2. temperatureThe mixture was cooled
  3. customthe solvent was decanted into ice-water (1 L)
  4. extractionThe product was extracted with ether
  5. washthe ethereal layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated in vacuo to an oil, which
  8. customwas used without further purification