HRID2351676

反应详情

EQUATION

反应方程式

HRID 2351676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under nitrogen bubbling, a mixture of 2-(4-chlorophenyl)-3H-imidazo [4,5-b]pyridine-3-acetic acid (4.0 g, 0.014 mole) and 1,1'-carbonyldiimidazole (2.27 g, 0.014 mole) in 150 ml of tetrahydrofuran was stirred at room temperature for 3 hours. Then, under nitrogen atmosphere, benzylamine (1.58 g, 0.0147 mole) was added and the reaction was allowed to stir at room temperature overnight. The tetrahydrofuran was evaporated, to give a solid. The solid was recrystallized from isopropyl alcohol, collected by filtration, washed with cold isopropyl alcohol and water, and dried under high vacuum at 50° C. overnight to give 3.43 g (65%) of title compound, mp 200°-200.5° C.

WORKUP

后处理

  1. stirringto stir at room temperature overnight
  2. customThe tetrahydrofuran was evaporated
  3. customto give a solid
  4. customThe solid was recrystallized from isopropyl alcohol
  5. filtrationcollected by filtration
  6. washwashed with cold isopropyl alcohol and water
  7. customdried under high vacuum at 50° C. overnight