HRID1924003

反应详情

EQUATION

反应方程式

HRID 1924003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

NaOH (6 M, 200 ml, 1200 mmole) was added to a solution of tert.-butyl 2-((1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methoxy)acetate (26.8 g, 62.7 mmole) in THF (200 ml) and methanol (200 ml). The reaction mixture was stirred at RT. After 1 hour the organic solvent was distilled off on a rotary evaporator and HCl (6 M, 210 ml) was added at 0° C. The aqueous phase was extracted with DCM (200 ml) and ethyl acetate (200 ml). The combined organic phases were dried over sodium sulfate and concentrated. Diisopropyl ether was added twice and evaporated. Yield: 21.92 g, 94%.

WORKUP

后处理

  1. distillationAfter 1 hour the organic solvent was distilled off on a rotary evaporator and HCl (6 M, 210 ml)
  2. additionwas added at 0° C
  3. extractionThe aqueous phase was extracted with DCM (200 ml) and ethyl acetate (200 ml)
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. concentrationconcentrated
  6. additionDiisopropyl ether was added twice
  7. customevaporated