HRID80867

反应详情

EQUATION

反应方程式

HRID 80867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 2-chloro-5-(4-chlorophenyl)pyridine (500 mg, 2.23 mmol), DMSO (2.0 mL) and 1-isopropylpiperazine (3 mL, 23.4 mmol) was stirred and heated on a 100° C. oil-bath overnight. The reaction mixture was poured into water (75 mL), and the solid was isolated by filtration, washed with water and dried. The crude product was purified by column chromatography on silica gel (Kiselgel 60, mesh 0.040-0.63) eluting with a mixture of ethyl acetate and methanol (4:1). Collecting the proper fractions afforded 600 mg (85%) of 1-[5-(4-chlorophenyl)pyridin-2-yl]-4-isopropylpiperazine.

WORKUP

后处理

  1. customthe solid was isolated by filtration
  2. washwashed with water
  3. customdried
  4. customThe crude product was purified by column chromatography on silica gel (Kiselgel 60, mesh 0.040-0.63)
  5. washeluting with a mixture of ethyl acetate and methanol (4:1)
  6. customCollecting the proper fractions