HRID2186187

反应详情

EQUATION

反应方程式

HRID 2186187 的结构方程式

PROCEDURE

实验过程

To a solution of 6-(tert-butoxycarbonyl)-1-oxa-6-azaspiro[2,5]octane (17.5 g) in methanol (250 ml) was added p-toluene sulfonic acid hydrate (285 mg), and the mixture was stirred at room temperature for 2 hours. The reaction solution was concentrated under reduced pressure, and to the residue was added ethyl acetate. The mixture was washed with sodium bicarbonate solution and saturated brine, dried and concentrated, and the residue was crystallized from ice-cooled hexane to give colorless solid of 1-(tert-butoxycarbonyl)-4-methoxy-4-piperidinemethanol (9.32 g).

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionto the residue was added ethyl acetate
  3. washThe mixture was washed with sodium bicarbonate solution and saturated brine
  4. customdried
  5. concentrationconcentrated
  6. customthe residue was crystallized from ice-
  7. temperaturecooled hexane