HRID2096992
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe DMSO was removed in vacuo
- additionA mixture of the residue and water (100 mL)
- extractionwas extracted with AcOEt (3×300 mL)
- extractionThe extractions
- washwashed with brine (300 mL)
- dry with materialdried over (Na2SO4)
- concentrationconcentrated