反应详情

To a suspension of sodium hydride (0.44 g) in N,N-dimethylformamide (10 ml) was added 5-ethyl-2-trifluoroacetylamino-1,3,4-thiadiazole (2.25 g) in three portions on ice. After the resulting mixture was stirred at the same temperature for 30 minutes, to the mixture was added 4-iodobenzyl bromide (2.97 g), and the mixture was stirred at room temperature for two hours. To the reaction mixture, ethyl acetate (50 ml) was added. The resulting mixture was washed successively with 10% aqueous citric acid solution and water and dried over anhydrous magnesium sulfate, followed by the removal through distillation. The residue so obtained was crystallized from n-hexane, collected by filtration and then dried, whereby 2.2 g of the title compound was obtained.

1. stirringthe mixture was stirred at room temperature for two hours
2. washThe resulting mixture was washed successively with 10% aqueous citric acid solution and water
3. dry with materialdried over anhydrous magnesium sulfate
4. customfollowed by the removal through distillation
5. customThe residue so obtained
6. customwas crystallized from n-hexane
7. filtrationcollected by filtration
8. customdried