HRID1388246

反应详情

EQUATION

反应方程式

HRID 1388246 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture (208.5 g) of the compound (X1) and the compound (X11) obtained in Step E was dissolved in ethanol (460 ml), and a solution of NaOH (28 g) and water (30 ml) was added and the mixture was heated, followed by reflux for one hour. After cooling, toluene (500 ml) and water (500 ml) were added, and the resulting toluene layer was washed with 2 N--NaOH aqueous solution and further with water till the layer became neutral. After removing toluene by concentration of the layer, the resulting raw crystals were recrystallized from ethyl acetate (130 ml) to obtain trans-4-(p-bromophenyl)-cyclohexanol (X11) (130 g) having a melting point of 109.5°~111.0° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureby reflux for one hour
  3. temperatureAfter cooling
  4. washthe resulting toluene layer was washed with 2 N
  5. customAfter removing toluene by concentration of the layer
  6. customthe resulting raw crystals were recrystallized from ethyl acetate (130 ml)