HRID127932

反应详情

EQUATION

反应方程式

HRID 127932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 36.5 g (0.2 mole) of γ-chlorobutyrophenone, 14 g of ethylene glycol (0.25 mole), 125 ml of toluene, and 0.1 g of p-toluenesulfonic acid is refluxed under a Dean-Stark trap for 1 hr. An additional 4 g of ethylene glycol is added and reflux continued for 3 hrs more. After cooling, the reaction mixture is washed with 5% sodium bicarbonate solution, dried with anhydrous magnesium sulfate, and concentrated. Upon standing at -10° C. overnight, the mixture partially crystallizes. The crystalline product is filtered and washed with petroleum ether to afford 17.7 g of 2-phenyl-2-(3'-chloropropyl)dioxolane, m.p. 56°-58°.

WORKUP

后处理

  1. temperatureis refluxed under a Dean-Stark trap for 1 hr
  2. temperaturereflux
  3. temperatureAfter cooling
  4. washthe reaction mixture is washed with 5% sodium bicarbonate solution
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. waitUpon standing at -10° C. overnight
  8. customthe mixture partially crystallizes
  9. filtrationThe crystalline product is filtered
  10. washwashed with petroleum ether