HRID621929

反应详情

EQUATION

反应方程式

HRID 621929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2-(4-bromophenyl)-3H-imidazo[4,5-b]pyridine-3-acetic acid (5.5 g, 0.0166 mole), 1,1'-carbonyldiimidazole (2.7 g, 0.0166 mole), and anhydrous tetrahydrofuran (100 ml) was stirred at room temperature with a stream of nitrogen bubbling through it for 21/2 hours. The nitrogen flow was stopped and a solution of dimethylamine (0.5M in tetrahydrofuran) (66 ml) was added. The solution was stirred at room temperature, stoppered, for 16 hours. The reaction mixture was concentrated in vacuo and the residue triturated in water (100 ml) and filtered. The filter cake was recrystallized from ethanol to give 3.78 g (;b 63%) of white needles, mp 224°-225° C.

WORKUP

后处理

  1. stirringThe solution was stirred at room temperature
  2. waitstoppered, for 16 hours
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. customthe residue triturated in water (100 ml)
  5. filtrationfiltered
  6. customThe filter cake was recrystallized from ethanol
  7. customto give 3.78 g (;b 63%) of white needles, mp 224°-225° C.