HRID982360

反应详情

EQUATION

反应方程式

HRID 982360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 1.02 g (3.2 mmol) of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride, 1.34 g of sodium hydrogencarbonate and 10 ml of dimethylformamide was stirred at 80° C. for 1 h. 0.48 g of 2-(2-chloroethyl)imidazo[1,2-a]pyridine hydrochloride and 0.53 g of potassium iodide were added thereto and the mixture was stirred at 80° C. for 2 h. The mixture was filtered and the filtrate was concentrated to obtain a solid residue, which was then purified according to silica gel column chromatography (chloroform:methanol:aqueous ammonia=190:9:1). The fraction of the intended compound was concentrated to obtain a solid residue, which was then recrystallized from ethyl acetate to obtain 0.25 g (yield: 18%) of the intended compound.

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. for 2 h
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated
  4. customto obtain a solid residue, which
  5. customwas then purified
  6. concentrationThe fraction of the intended compound was concentrated
  7. customto obtain a solid residue, which
  8. customwas then recrystallized from ethyl acetate