HRID1056632

反应详情

EQUATION

反应方程式

HRID 1056632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of tert-butyl 5-(benzylamino)hexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate (6.50 g, 20.5 mmol) and AcOH (1.23 g, 20.5 mmol) in MeOH (150 mL) was added Pd(OH)2/C (10% wt, 1.00 g), and the suspension was stirred at 40° C. under H2 atmosphere overnight. The mixture was filtered through a pad of Celite and then concentrated in vacuo. The residue was dissolved in saturated NaHCO3 solution (70 mL) and extracted with DCM (100 mL×3). The combined organic phases were washed with brine (100 mL×3), dried over anhydrous Na2SO4, then filtered and concentrated in vacuo to give the title compound as a yellow solid (4.00 g, 86.2%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a pad of Celite
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in saturated NaHCO3 solution (70 mL)
  4. extractionextracted with DCM (100 mL×3)
  5. washThe combined organic phases were washed with brine (100 mL×3)
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo