HRID272231

反应详情

EQUATION

反应方程式

HRID 272231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 3.82 g (10 mmol) of tert-butyl trans-benzyl[4-(4-hydroxyphenyl)-cyclohexyl]carbamate (cf. preparation 1.2) and of 0.48 g of 60% sodium hydride (12 mmol) in dimethylformamide (38 ml) is stirred for 25 minutes and then 1.44 ml of ethyl bromoacetate (13 mmol) are added. The reaction is left stirring for 4 h. The reaction medium is neutralized by the addition of a saturated aqueous ammonium chloride solution. The solvents are evaporated under reduced pressure and water and dichloromethane are added. The organic phase is washed 5 times with water and then dried over magnesium sulfate. Ethyl trans-(4-{4-[benzyl(tert-butoxycarbonyl)amino]cyclohexyl}phenoxy)acetate is obtained in the form of a white solid (4.68 g, 100%) after evaporation of the solvents under reduced pressure.

WORKUP

后处理

  1. waitThe reaction is left
  2. customThe solvents are evaporated under reduced pressure and water and dichloromethane
  3. additionare added
  4. washThe organic phase is washed 5 times with water
  5. dry with materialdried over magnesium sulfate