HRID46474

反应详情

EQUATION

反应方程式

HRID 46474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 100 g of indanone, 112 g of p-chlorobenzaldehyde and 500 ml of ethanol is stirred, the resulting solution is cooled to -10° and treated rapidly (3 minutes) with a solution of 5.0 g of KOH in 100 ml of ethanol. The solution is allowed to warm and the product begins to crystallize at 17° (cooled to keep under 15°). The resulting slurry is allowed to stir at 20°-25° for 1 hour, and then poured onto 2 liters of icewater. After standing for 3 hours, the solid is filtered, washed with cold water and allowed to air dry; wt., 190 g, m.p. 174°-179°. After crystallization from 400 ml of DMF, the cream-colored solid weighs 164.5 g (86%), m.p. 177°-179°.

WORKUP

后处理

  1. temperaturethe resulting solution is cooled to -10°
  2. temperatureto warm
  3. customto crystallize at 17°
  4. temperature(cooled to keep under 15°)
  5. stirringto stir at 20°-25° for 1 hour
  6. additionpoured onto 2 liters of icewater
  7. filtrationthe solid is filtered
  8. washwashed with cold water
  9. customto air dry
  10. customAfter crystallization from 400 ml of DMF