HRID5446
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 solution of 5-[2-(hydroxy)ethylthio]imidazo[1,2-a]pyridine (971 mg, 5 mmoles) and trietylamine (0.91 ml, 6.53 mmoles) in methylene chloride (40 ml) was added methyl isocyanate (0.65 ml, 11 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 12 hours. The reaction mixture was washed with saturated saline and dried over anhydrous magnesium sulfater. After the solvent was distilled off, the residue was purified by column chromatography (eluent: methanol/chloroform=1:20) to obtain 1.07 g of the desired product (85.2%, colorless crystals).
WORKUP
后处理
- temperaturecooling
- stirringthe mixture was stirred at room temperature for 12 hours
- washThe reaction mixture was washed with saturated saline
- dry with materialdried over anhydrous magnesium sulfater
- distillationAfter the solvent was distilled off
- customthe residue was purified by column chromatography (eluent: methanol/chloroform=1:20)