HRID1816715

反应详情

EQUATION

反应方程式

HRID 1816715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[3-(methanesulfonyloxy)propyloxy]-N-t-butyloxycarbonylpiperidine (3.76 g) in methanol (20 ml) was added 28% sodium methoxide methanol solution (22.7 ml), and the mixture was stirred under refluxing for 1.5 hours. The reaction mixture was evaporated in vacuo and dissolved in ethyl acetate (200 ml). The solution was washed twice with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and evaporated in vacuo. The resulting residue was chromatographed on silica gel (200 ml) eluting with a mixture of n-hexane and ethyl acetate (2:1 v/v). The fractions containing the object compound were collected and evaporated under reduced pressure to give 4-(3-methoxypropyloxy)-N-t-butyloxycarbonylpiperidine (2.66 g).

WORKUP

后处理

  1. temperatureunder refluxing for 1.5 hours
  2. customThe reaction mixture was evaporated in vacuo
  3. dissolutiondissolved in ethyl acetate (200 ml)
  4. washThe solution was washed twice with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customThe resulting residue was chromatographed on silica gel (200 ml)
  8. washeluting with a mixture of n-hexane and ethyl acetate (2:1 v/v)
  9. additionThe fractions containing the object compound
  10. customwere collected
  11. customevaporated under reduced pressure