HRID1372587

反应详情

EQUATION

反应方程式

HRID 1372587 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 methyl (2S,4S)-1-tert-butoxycarbonyl-4-phenoxy-2-pyrrolidinylcarboxylate (5.31 g, 16.5 mmol) in THF (132 ml) was added 0.25N NaOH (132 ml, 33.0 mmol). The reaction mixture was stirred overnight at room temperature. The residue obtained by concentrating the reaction mixture under reduced pressure was acidified with 1N HCl, followed by extraction with chloroform. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent. The crude crystals thus obtained were recrystallized from hexane-chloroform, whereby the title compound (2.96 g, 58%) was obtained as a white crystalline powder.

WORKUP

后处理

  1. customThe residue obtained
  2. concentrationby concentrating the reaction mixture under reduced pressure
  3. extractionfollowed by extraction with chloroform
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent
  8. customThe crude crystals thus obtained
  9. customwere recrystallized from hexane-chloroform, whereby the title compound (2.96 g, 58%)
  10. customwas obtained as a white crystalline powder