HRID1657514

反应详情

EQUATION

反应方程式

HRID 1657514 反应方程式

PROCEDURE

实验过程

To an ethereal solution of n-propyl magnesium iodide (prepared from 0.07 molar n-propyl iodide and magnesium in 100 ml. ether) was added, while stirring, a solution of 16.9 g. (0.05 mole) α-trifluoroethyl-deoxyanisoin (see Example 1a)) and the reaction mixture was heated under reflux for 3 hours, whereafter it was poured into ice - dilute hydrochloric acid and extracted with ether. The ethereal extract was washed with water and an aqueous solution of sodium bisulphite, dried and evaporated to dryness. There was obtained an oily residue of 4,4'-dimethoxy-α-(n-propyl)-α-hydroxy-α'-trifluoroethyl-bibenzyl.

WORKUP

后处理

  1. temperatureunder reflux for 3 hours, whereafter it
  2. additionwas poured into ice - dilute hydrochloric acid
  3. extractionextracted with ether
  4. extractionThe ethereal extract
  5. washwas washed with water
  6. dry with materialan aqueous solution of sodium bisulphite, dried
  7. customevaporated to dryness