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 200 ml of dichloromethane are added 10.0 g (0.043 mole) of 2-chloroimidazo[1,2-a]pyridine-3sulfonamide and 8.85 g (0.0866 mole) of triethylamine, followed by adding dropwise 6.78 g (0.0433 mole) of phenyl chloroformate with stirring at 20° to 25° C. The mixture is further stirred at the same temperature for 30 minutes, and 4.20 g (0.0433 mole) of 2-amino-4,6-dimethoxyacid and 6.72 g (0.0433 mole) of 2-amino-4,6-dimethoxypyrimidine are added to the mixture in that order. The mixture is refluxed for 5 hours. After completion of the reaction, the dichloromethane is removed under reduced pressure and to the residue is added 50 ml of acetonitrile. The resulting crystals are collected by filtration, washed with three 10 ml portions of acetonitrile and water with water. The crystals were dried in vacuo over P2O5 to give 15.62 g (yield 87.9%) of the title compound.
WORKUP
后处理
- stirringThe mixture is further stirred at the same temperature for 30 minutes
- temperatureThe mixture is refluxed for 5 hours
- customAfter completion of the reaction
- customthe dichloromethane is removed under reduced pressure and to the residue
- additionis added 50 ml of acetonitrile
- filtrationThe resulting crystals are collected by filtration
- washwashed with three 10 ml portions of acetonitrile and water with water
- dry with materialThe crystals were dried in vacuo over P2O5