HRID1361240

反应详情

EQUATION

反应方程式

HRID 1361240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of [(S)-1-(2-carbamoyl-pyridin-4-yl)-propyl]carbamic acid tert-butyl ester (1 g, 3.58 mmol) in MeOH (16.6 mL) and glacial acetic acid (3.3 mL) was added to a flask containing 10% palladium on carbon (0.38 g, 0.36 mmol) under nitrogen. The reaction was stirred at 60° C. under hydrogen at 400 psi using a Biotage Endeavour Argonaut instrument. After 20 hours, the reaction was filtered and concentrated. The crude material was diluted with EtOAc (100 mL), washed with saturated sodium carbonate solution (20 mL), brine, dried over sodium sulfate, filtered and concentrated to afford [(S)-1-(2-carbamoyl-piperidin-4-yl)-propyl]carbamic acid tert-butyl ester as a white solid.

WORKUP

后处理

  1. filtrationthe reaction was filtered
  2. concentrationconcentrated
  3. additionThe crude material was diluted with EtOAc (100 mL)
  4. washwashed with saturated sodium carbonate solution (20 mL), brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated