HRID216064

反应详情

EQUATION

反应方程式

HRID 216064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-tert-Butyl 4-ethyl 4-((2-methoxyethoxy)methyl)piperidine-1,4-dicarboxylate from step A (1.78 g, 5.15 mmol) was treated with LiOH (0.62 g. 26 mmol) in ethanol (12 mL) and water (24 mL) at 80° C. for 18 hours. The mixture was cooled, diluted with dichloromethane, and washed with sat. aq. NaHSO4. The aqueous phase was back extracted with dichloromethane (3×), and the organics were combined, washed with brine, dried over MgSO4, and concentrated to give the title compound in quantitative yield. MS (ES+) [M+H]+=318.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. washwashed with sat. aq. NaHSO4
  3. extractionThe aqueous phase was back extracted with dichloromethane (3×)
  4. washwashed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated