HRID857095

反应详情

EQUATION

反应方程式

HRID 857095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(1R)-2-Azido-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)ethanol (16.99 g) was hydrogenated over 10% Pd—C (1 g) in EtOH (300 ml). The catalyst was collected by filtration, and washed with EtOH. The combined washings were evaporated under reduced pressure and the residue was triturated in ether to give the title compound (5.86 g). The mother liquors were chromatographed on a Biotage column eluting with toluene:EtOH:aqueous ammonia (85:14:1) to give a further batch of the title compound (5.99 g). LCMS RT=1.68 min, ES+ve 206 (MH—H2O)+.

WORKUP

后处理

  1. filtrationThe catalyst was collected by filtration
  2. washwashed with EtOH
  3. customThe combined washings were evaporated under reduced pressure
  4. customthe residue was triturated in ether