HRID364621

反应详情

EQUATION

反应方程式

HRID 364621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This example serves to illustrate procedure B of Scheme 2. To an ice-cooled solution of 1-(2-pyrimidinyl)piperazine (16.4 g, 0.1 mole) in 1N HCl (100 mL) was added dropwise bromine (15.98 g, 0.1 mole). After stirring at 0° for 0.5 hr, the mixture was heated to 100° until dissipation of the red color had occurred. The mixture is filtered, cooled, made alkaline with 50% NaOH and extracted with ether. The dried extract (MgSO4) was concentrated in vacuo to provide 14.5 g (62%) of product, m.p. 73°-75°.

WORKUP

后处理

  1. temperaturethe mixture was heated to 100° until dissipation of the red color
  2. filtrationThe mixture is filtered
  3. temperaturecooled
  4. extractionextracted with ether
  5. extractionThe dried extract (MgSO4)
  6. concentrationwas concentrated in vacuo