HRID2096992

反应详情

EQUATION

反应方程式

HRID 2096992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
18 °C

PROCEDURE

实验过程

A stirred solution of 5,7-Dichloroimidazo[4,5-b]pyridine (5 g, 26.5 mmol.) in DMSO (50 mL) was cooled in an ice bath, and treated with K2CO3 (14.6 g, 106.2 mmol.) and 2-bromopropane (12.47 mL, 132.8 mmol.). The mixture was allowed to warm to 18° C. and stirred overnight. The DMSO was removed in vacuo. A mixture of the residue and water (100 mL) was extracted with AcOEt (3×300 mL). The extractions were combined, washed with brine (300 mL), dried over (Na2SO4) and concentrated. Chromatography of the residue on silica gel with toluene-AcOEt-CH2Cl2 3:1:1 gave 5,7-Dichloro-3-iso-propylimidazo[4,5-b]pyridine. (Yield: 57%).

WORKUP

后处理

  1. customThe DMSO was removed in vacuo
  2. additionA mixture of the residue and water (100 mL)
  3. extractionwas extracted with AcOEt (3×300 mL)
  4. extractionThe extractions
  5. washwashed with brine (300 mL)
  6. dry with materialdried over (Na2SO4)
  7. concentrationconcentrated