HRID2407847

反应详情

EQUATION

反应方程式

HRID 2407847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Diethyl 3-azidopropylphosphonate (1 eq) was dissolved in EtOH (0.1 M). Pd(OH)2 (0.02 eq) was added to the reaction. Hydrogen gas was introduced via a balloon and the reaction was stirred for 3 hours. The reaction was stirred for for a further 2 hours at room temperature and filtered through Celite and washed with methanol. The solvent was removed en vaccuo and the crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-10% MeOH in DCM with 0.5% NH3 in MeOH to give the product as colorless oil.

WORKUP

后处理

  1. stirringThe reaction was stirred for for a further 2 hours at room temperature
  2. filtrationfiltered through Celite
  3. washwashed with methanol
  4. customThe solvent was removed en vaccuo
  5. customthe crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO)