HRID1461951

反应详情

EQUATION

反应方程式

HRID 1461951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

128 g of 3,5-dimethyl-cyclohexanol and 500 ml of benzene are added to a round flask which is fitted with a stirrer, thermometer, dropping funnel and reflux condenser. While stirring and cooling there is now slowly added dropwise thereto a mixture of 119 g of sodium dichromate, 500 ml of water, 162 ml of concentrated sulphuric acid and 50 ml of glacial acetic acid. Thereby the temperature should not exceed +10° C. The mixture is stirred at this temperature for a further 3 hours and then the organic phase is separated. The aqueous phase is diluted with 130 ml of water and extracted with benzene. The combined organic phases are washed neutral and concentrated. The residue is distilled over a Widmer column and gives 102.7 g of 3,5-dimethyl-cyclohexanone.

WORKUP

后处理

  1. customis fitted with a stirrer
  2. temperaturereflux condenser
  3. temperaturecooling there
  4. additionis now slowly added dropwise
  5. customexceed +10° C
  6. stirringThe mixture is stirred at this temperature for a further 3 hours
  7. customthe organic phase is separated
  8. additionThe aqueous phase is diluted with 130 ml of water
  9. extractionextracted with benzene
  10. washThe combined organic phases are washed neutral
  11. concentrationconcentrated
  12. distillationThe residue is distilled over a Widmer column