HRID1658564

反应详情

EQUATION

反应方程式

HRID 1658564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 43.5 parts of magnesium in 125 parts by volume of ether is added a portion of a solution containing 84 parts of methyl cyclohexylmethyl ketone and 71.4 parts of propargyl bromide in a solution consisting of 60 parts by volume of benzene and 180 parts by volume of ether. After the addition of 0.05 part of mercuric chloride to initiate the reaction, the remainder of the reactants is added dropwise. The reaction mixture is heated at the reflux temperature for about 15 minutes, allowed to cool to room temperature, then poured carefully into cold dilute hydrochloric acid. The aqueous phase is separated, extracted with ether and the combined ether extracts are washed successively with water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate and evaporated to dryness. Vacuum distillation of the residue affords 4(RS)-4-cyclohexylmethyl-4-methyl-1-butyn-4-ol.

WORKUP

后处理

  1. additionis added a portion of a solution
  2. customthe reaction
  3. additionthe remainder of the reactants is added dropwise
  4. temperatureThe reaction mixture is heated at the reflux temperature for about 15 minutes
  5. customThe aqueous phase is separated
  6. extractionextracted with ether
  7. washthe combined ether extracts are washed successively with water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated to dryness
  10. distillationVacuum distillation of the residue