HRID1978351
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of ethyl (imidazo[1,2-a]pyridin-5-ylthio)acetate (11.8 g) in acetic acid (120 ml) was added hexamethylenetetramine (14.0 g) and the mixture was reacted at 90° C. for 10 hours. After this reaction mixture was allowed to cool, ethyl acetate (360 ml) was added and the mixture was washed with water. The organic layer was neutralized with 30% aqueous solution of sodium hydroxide under ice-cooling and washed again with water. The organic layer was concentrated and n-hexane (100 ml) was added to the crystalline residue, followed by 1 hour of stirring at room temperature. The crystals were collected by filtration and dried to provide the title compound (9.6 g, 78%).
WORKUP
后处理
- customthe mixture was reacted at 90° C. for 10 hours
- temperatureto cool
- washthe mixture was washed with water
- temperaturecooling
- washwashed again with water
- concentrationThe organic layer was concentrated
- additionn-hexane (100 ml) was added to the crystalline residue
- filtrationThe crystals were collected by filtration
- customdried