HRID1085659

反应详情

EQUATION

反应方程式

HRID 1085659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2.4 ml (19.5 mmol) of isovaleric acid chloride are added dropwise at 0° C. to a solution of 2 75 g (17.76 mmol) of 1-cyclohexyl-3-buten-2-ol, 3 ml (21.3 mmol) of triethylamine and 430 mg (3.5 mmol) of 4-dimethylaminopyridine in 20 ml of methylene chloride. When the addition is complete, the mixture is stirred for a further 3 hours at room temperature. After diluting with ether, the mixture is washed twice with 2N HCl, twice with saturated NaHCO3 solution and twice with brine and dried over MgSO4. After concentration by evaporation, the residue is distilled in a bulb tube at 150°/0.007 mbar.

WORKUP

后处理

  1. additionWhen the addition
  2. washthe mixture is washed twice with 2N HCl, twice with saturated NaHCO3 solution and twice with brine
  3. dry with materialdried over MgSO4
  4. concentrationAfter concentration
  5. customby evaporation
  6. distillationthe residue is distilled in a bulb tube at 150°/0.007 mbar