HRID2051405

反应详情

EQUATION

反应方程式

HRID 2051405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

53 Grams of 60% sodium hydride was gradually added to a solution prepared by dissolving 256.2 g of cyclohexyl 3,5-dimethyl-2-hydroxyphenyl ketone in 1 liter of dimethylformamide with stirring, generating the temperature of the reaction mixture was risen to 70° C. by generating the heat. After continuation of stirring for 30 minutes, the reaction mixture was cooled to room temperature and thereto was added dropwise 233 g of methyl iodide. The reaction mixture was further stirred at the same temperature for 2 hours and then added to 1 liter of ice water and stirred. The organic layer was extracted with 3 liters of ethyl acetate. The extract was washed with water and then with a saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 285.2 g of cyclohexyl 3,5-dimethyl-2-methoxyphenyl ketone.

WORKUP

后处理

  1. customprepared
  2. customwas risen to 70° C.
  3. stirringAfter continuation of stirring for 30 minutes
  4. stirringThe reaction mixture was further stirred at the same temperature for 2 hours
  5. stirringstirred
  6. extractionThe organic layer was extracted with 3 liters of ethyl acetate
  7. washThe extract was washed with water
  8. dry with materialwith a saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate
  9. distillationThe solvent was distilled off under reduced pressure