HRID659017

反应详情

EQUATION

反应方程式

HRID 659017 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2.90 g (9.41 mmol) 3-[4-(2-fluoro-4-nitro-phenoxy)-pyrimidin-2-ylamino]-propan-1-ol in a mixture of 50 ml TH/methanol 1:1 was hydrogenated over 500 mg 10% Pd/C for 10 h. The catalyst was filtered off and the filtrate evaporated. The obtained oil was dissolved in ethyl acetate and purified by chromatography on silica (dichloromethane/methanol 94:6) to give 1.70 g (65%) of 3-[4-(4-amino-2-fluoro-phenoxy)-pyrimidin-2-ylamino]-propan-1-ol.

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate evaporated
  3. dissolutionThe obtained oil was dissolved in ethyl acetate
  4. custompurified by chromatography on silica (dichloromethane/methanol 94:6)