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
PROCEDURE
实验过程
To a stirred mixture of 6-chloro-imidazo[1,2-b]pyridazine-2-carboxylic acid [5-(3-trifluoromethyl-phenyl)-1H-benzoimidazol-2-yl]-amide (100 mg) and 2-morpholin-4-yl-ethanol (250 μL) in dry DMF (1 mL) was added NaH (100 mg, 60% dispersion in mineral oil) and the mixture was stirred at room temperature for 1 h. To this was added water (20 mL) and the reaction mixture stirred for 10 minutes. The precipitated solid was filtered and purified by column chromatography (12 g pre-packed silica gel column cartridge) using DCM and 2N ammonia in methanol to afford 6-(2-morpholin-4-yl-ethoxy)-imidazo[1,2-b]pyridazine-2-carboxylic acid [5-(3-trifluoromethyl-phenyl)-1H-benzoimidazol-2-yl]-amide (42 mg). LCMS (m/z): 552.8.
WORKUP
后处理
- stirringthe reaction mixture stirred for 10 minutes
- filtrationThe precipitated solid was filtered
- custompurified by column chromatography (12 g pre-packed silica gel column cartridge)