HRID1800827

反应详情

EQUATION

反应方程式

HRID 1800827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Tert-butyl 4-(aminomethyl)-4-phenylpiperidine-1-carboxylate (355 mg, 1.22 mmol) and 1.15 g PtO2 (5.1 mmol) in 125 ml ethanol were shaked in PARR apparatus under 60 psi of hydrogen for 20 hours. Celite was loaded on top of an ion exchange cartridge (MCX, Phenomenex, 6 g adsorbent). The crude reaction slurry was filtered through this set-up, the pyrophoric catalyst washed with ethanol and water and removed. The cartridge was washed with methanol and then the product eluted with a 2 M solution of NH3 in MeOH. The eluent was concentrated to give 234 mg of the title compound as an oil.

WORKUP

后处理

  1. customThe crude reaction slurry
  2. filtrationwas filtered through this set-up
  3. washthe pyrophoric catalyst washed with ethanol and water
  4. customremoved
  5. washThe cartridge was washed with methanol
  6. washthe product eluted with a 2 M solution of NH3 in MeOH
  7. concentrationThe eluent was concentrated