HRID635059

反应详情

EQUATION

反应方程式

HRID 635059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, lithium aluminum hydride (381 mg, 9.54 mmol) was suspended in anhydrous tetrahydrofuran (30 ml) to which, while cooling in an ice bath, was subsequently added dropwise an anhydrous tetrahydrofuran (10 ml) solution of ethyl trans-1-benzyl-4-(1-tert-butoxycarbonylaminocyclopropyl)pyrrolidine-3-carboxylate (1.24 g, 3.18 mmol) over a period of 15 minutes. After 4 hours of stirring at the same temperature, ice-cooled water was gradually added to the reaction solution. The reaction suspension was subjected to celite filtration (chloroform washing) to separate the organic layer. The aqueous layer was extracted with chloroform (50 ml×2), and the organic layers were combined and dried over anhydrous sodium sulfate. By evaporating the solvent, 1.12 g (>99%) of the title compound was obtained.

WORKUP

后处理

  1. temperaturewhile cooling in an ice bath
  2. additionwas gradually added to the reaction solution
  3. filtrationThe reaction suspension was subjected to celite filtration (chloroform washing)
  4. customto separate the organic layer
  5. extractionThe aqueous layer was extracted with chloroform (50 ml×2)
  6. dry with materialdried over anhydrous sodium sulfate
  7. customBy evaporating the solvent