反应详情

To a suspension of sodium hydride (4.4 g) in N,N-dimethylformamide (100 ml) was added 5-ethyl-2-trifluoroacetylamino-1,3,4-thiadiazole (24 g) in three portions on ice. After stirring at the same temperature for 30 minutes, to the resulting mixture was added 4-bromobenzyl bromide (25 g), followed by stirring at room temperature for one hour. To the reaction mixture, ethyl acetate (500 ml) was added. The resulting mixture was washed successively with 10% aqueous citric acid solution and water and was dried over anhydrous magnesium sulfate, followed by removal through distillation. The residue so obtained was dispersed in a 2:3 mixed solvent of diisopropyl ether and n-hexane, collected by filtration and then dried, whereby 24.8 g of the title compound was obtained.

1. stirringby stirring at room temperature for one hour
2. washThe resulting mixture was washed successively with 10% aqueous citric acid solution and water
3. dry with materialwas dried over anhydrous magnesium sulfate
4. customfollowed by removal through distillation
5. customThe residue so obtained
6. filtrationcollected by filtration
7. customdried