HRID1157042

反应详情

EQUATION

反应方程式

HRID 1157042 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

6.7 -Dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one(63.5 gm., 0.274 mole) is dissolved in a mixture of dry tert.-butyl alcohol (500 ml.) and dry benzene (1.5 liters). The solution is refluxed and potassium tert.-butoxide (46 gm., 0.301 mole) in dry tert.-butyl alcohol (1 liter) is added as rapidly as possible. The solution is refluxed for another 1/2 hour, cooled to 20° C., stirred and treated with allyl bromide (36 gm., 0.301 mole). The mixture is stirred and refluxed for 4 hours, cooled and treated with water (250 ml.). The crude 2-allyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one is separated by filtration, washed with water, dried and recrystallized from a mixture of benzene and hexane.

WORKUP

后处理

  1. temperatureThe solution is refluxed
  2. temperatureThe solution is refluxed for another 1/2 hour
  3. stirringThe mixture is stirred
  4. temperaturerefluxed for 4 hours
  5. temperaturecooled
  6. customThe crude 2-allyl-6,7-dichloro-5-methoxy-2,3-dihydro-1H-inden-1-one is separated by filtration
  7. washwashed with water
  8. customdried
  9. customrecrystallized from a mixture of benzene and hexane