HRID276772

反应详情

EQUATION

反应方程式

HRID 276772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-Chloro-5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridine (72.8 g) and piperazine (61.8 g) in DMSO (478 mL) was heated to 105 degrees 16 hours. The reaction mixture was cooled to room temperature and diluted with 2500 mL half-saturated brine. The resultant precipitate was collected by filtration and triturated with 2000 mL hot methanol. The solids were collected by filtration, the mother liquor was concentrated to about 100 mL, and the additional precipitate was collected and combined with the original solids to provide 1-{5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridin-2-yl}-piperazine (49 g).

WORKUP

后处理

  1. filtrationThe resultant precipitate was collected by filtration
  2. customtriturated with 2000 mL hot methanol
  3. filtrationThe solids were collected by filtration
  4. concentrationthe mother liquor was concentrated to about 100 mL
  5. customthe additional precipitate was collected