HRID28114

反应详情

EQUATION

反应方程式

HRID 28114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Sodium (5.7 g) is dissolved in ethanol (160 cc), and a solution of para-cresol (27 g) in ethanol (20 cc) is added. The mixture is stirred for 1 hour at 20° C. and ethyl dichloroacetate (20 g) in solution in ethanol (20 cc) is then added. The mixture is heated under reflux for 20 hours and then allowed to cool. The white precipitate obtained is filtered off and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil thus obtained is taken up in diethyl ether (300 cc) and washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time). The ethereal phase is then dried over anhydrous sodium sulphate, filtered, and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylphenoxy)acetate (29 g) is thus obtained as a yellow oil.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 20 hours
  3. temperatureto cool
  4. customThe white precipitate obtained
  5. filtrationis filtered off
  6. concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
  7. customThe oil thus obtained
  8. washwashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
  9. dry with materialThe ethereal phase is then dried over anhydrous sodium sulphate
  10. filtrationfiltered
  11. concentrationconcentrated to dryness under reduced pressure (20 mmHg) at 40° C