HRID46624

反应详情

EQUATION

反应方程式

HRID 46624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 25 g. (0.181 mole) of 3,4-methylenedioxyphenol, 36 g. (0.181 mole) of α-bromoacetophenone and 41.2 g. (0.40 mole) of sodium carbonate in 350 ml. of benzene is heated to its reflux temperature and maintained at reflux for 16 hours. To the mixture is added 50 g. of potassium carbonate, and the mixture is refluxed for an additional 7 days while collecting water in a Barrett water trap. The mixture is then diluted with a mixture of water and benzene. The benzene layer is washed with water, then cold 5 percent sodium hydroxide solution. A precipitate forms in the benzene layer. It is collected, rinsed with benzene and dried to provide a white powder which is recrystallized from ethanol to provide α-(3,4-methylenedioxyphenoxy)acetophenone, m.p. 123°-126° C.

WORKUP

后处理

  1. additionA mixture of 25 g
  2. temperaturereflux temperature
  3. temperaturemaintained
  4. temperatureat reflux for 16 hours
  5. additionTo the mixture is added 50 g
  6. customwhile collecting water in a Barrett water trap
  7. additionThe mixture is then diluted with a mixture of water and benzene
  8. washThe benzene layer is washed with water
  9. customIt is collected
  10. washrinsed with benzene
  11. customdried
  12. customto provide a white powder which
  13. customis recrystallized from ethanol