HRID2289527

反应详情

EQUATION

反应方程式

HRID 2289527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(Benzyl)-4-(4-chloropyrimidin-6-yl)piperazine (58.0 g) was dissolved, with some heating, in methanol (700 ml), treated with 10% Pd on activated carbon (11.6 g) and agitated and hydrogenated at atmospheric pressure for 8 h. The catalyst was removed by filtering through celite. The filtrate thus obtained was then evaporated under reduced pressure to a yellow-brown viscous gum which was chromatographed through 60 υm silica gel, eluting with 5% methanol, 1% ammonium hydroxide and 94% dichloromethane to obtain 4-(4-pyrimidinyl)piperazine, as a white solid, 25 g (76% yield based on prehydrogenation substrate);

WORKUP

后处理

  1. customThe catalyst was removed
  2. filtrationby filtering through celite
  3. customThe filtrate thus obtained
  4. customwas then evaporated under reduced pressure to a yellow-brown viscous gum which
  5. customwas chromatographed through 60 υm silica gel
  6. washeluting with 5% methanol, 1% ammonium hydroxide and 94% dichloromethane