HRID491640

反应详情

EQUATION

反应方程式

HRID 491640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(3,4-Dinitro-phenoxy)-2-methylsulfanyl-pyrimidine (Step A, 1.0 g, 3.2 mmol, 1.0 eq.) was dissolved in MeOH (10 mL) and the atmosphere was replaced by argon. A catalytic amount of 10% Pd/C was added and the argon was replaced by a H2 atmosphere. The mixture was hydrogenated for 2 h at RT at 60 psi using a Parr hydrogenation apparatus. More Pd/C was added and the mixture was hydrogenated for another 4 h at 60 psi. The Pd/C was removed by filtration. The crude aniline was purified using column chromatography (0-100% EtOAc in hexanes) to give 4-(2-methylsulfanyl-pyrimidin-4-yloxy)-benzene-1,2-diamine.

WORKUP

后处理

  1. waitthe mixture was hydrogenated for another 4 h at 60 psi
  2. customThe Pd/C was removed by filtration
  3. customThe crude aniline was purified