HRID898777

反应详情

EQUATION

反应方程式

HRID 898777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of benzyl 7-[(2S)-2-[(tert-butoxycarbonyl)amino]-3-(4-cyanophenoxy)propyl]-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (from step (ix) above; 2.55 g, 4.7 mmol) in 95% ethanol (50 mL) was hydrogenated over 5% Pd/C (0.8 g) at 30 kPa. When the quantity of hydrogen calculated for complete reaction had been consumed, the reaction was stopped. The mixture was filtered through Celite®, and the filtrate concentrated in vacuo. The resulting residue was purified by chromatography on silica, eluting with CHCl3:ammoniacal methanol (95:5), to yield the title compound 1.39 g (75%).

WORKUP

后处理

  1. customhad been consumed
  2. filtrationThe mixture was filtered through Celite®
  3. concentrationthe filtrate concentrated in vacuo
  4. customThe resulting residue was purified by chromatography on silica
  5. washeluting with CHCl3