HRID1032410

反应详情

EQUATION

反应方程式

HRID 1032410 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

38.16 g (0.2 mol) of p-toluenesulphonyl chloride are added at room temperature while stirring to a solution of 31 g (0.189 mol) of 2-hydroxymethylchroman in 110 ml of absolute pyridine, the slightly exothermic reaction being maintained at room temperature by means of an ice bath. The reaction mixture is stirred for a further 3 hours at room temperature and then poured onto ice-water. The oil which separates out is removed by decanting the aqueous phase, dissolved in diethyl ether and washed with ice-cold 2N hydrochloric acid and ice-water. The ethereal phases are dried over sodium sulphate and concentrated by evaporation in vacuo. 58.15 g (96.6%) of 2-(p-toluenesulphonyloxymethyl)chroman are obtained in the form of a colourless oil.

WORKUP

后处理

  1. customthe slightly exothermic reaction
  2. additionpoured onto ice-water
  3. customThe oil which separates out is removed
  4. customby decanting the aqueous phase
  5. dissolutiondissolved in diethyl ether
  6. washwashed with ice-cold 2N hydrochloric acid and ice-water
  7. dry with materialThe ethereal phases are dried over sodium sulphate
  8. concentrationconcentrated by evaporation in vacuo