HRID399126

反应详情

EQUATION

反应方程式

HRID 399126 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 1-(t-butoxycarbonyl)piperidine-3(S)-carboxylate (35.9 g, 0.099 mol) was dissolved in abs EtOH (70 mL), treated with 0.5N NaOH (418 mL, 0.209 mol), and heated at reflux for 0.75 h. The reaction mixture was cooled and extracted with EtOAc. The aqueous basic layer was cooled with ice, carefully acidified (pH 3) with 3N HCl and extracted with CH2 Cl2 (3×100 mL). The organics were combined, dried (MgSO4), filtered, and concentrated to give the title compound.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 0.75 h
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with EtOAc
  5. temperatureThe aqueous basic layer was cooled with ice
  6. extractionextracted with CH2 Cl2 (3×100 mL)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated