HRID1955002

反应详情

EQUATION

反应方程式

HRID 1955002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

0.88 ml (7.85 mmol) of 4-chlorobutyryl chloride is added dropwise at 0-5° C. with stirring to a solution of 2.2 g (7.85 mmol) of 8-(2-amino-6-methylbenzylamino)-2,3-dimethylimidazo[1,2-a]pyridine and 0.63 ml (7.85 mmol) of pyridine in 30 ml of dichloromethane and the mixture is stirred for a further 2 h at 0-20° C. It is treated with water and potassium hydrogen carbonate to pH 7, the mixture is extracted with shaking, and the organic layer is dried with magnesium sulfate and concentrated in vacuo. The residue is recrystallized from toluene and petroleum ether (50/70° C.). 2.6 g (86%) of the title compound are obtained. M.p. 138-140° C.

WORKUP

后处理

  1. extractionthe mixture is extracted
  2. stirringwith shaking
  3. dry with materialthe organic layer is dried with magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is recrystallized from toluene and petroleum ether (50/70° C.)