反应详情

To a stirred suspension of 3.3 g of 2-amino-5-(1-ethyl-1-methylpropyl)-1,3,4-thiadiazole in 30 ml of tetrahydrofuran were added in one portion 2.8 g of benzoyl chloride. The reaction mixture was stirred at room temperature while a solution of 1.6 g of pyridine in 20 ml of tetrahydrofuran was added dropwise over thirty minutes. Following complete addition, the reaction mixture was heated at reflux for three hours. The mixture was then filtered to remove the pyridine hydrochloride, and the filtrate was washed several times with 1N hydrochloric acid solution. The organic layer was separated and the solvent was removed by evaporation under reduced pressure to provide a yellow gum. The gum was crystallized from ethanol and water to afford 1.85 g of N-[5-(1-ethyl-1-methylpropyl)-1,3,4-thiadiazol-2-yl]benzamide.

1. additionwas added dropwise over thirty minutes
2. additionaddition
3. temperaturethe reaction mixture was heated
4. temperatureat reflux for three hours
5. filtrationThe mixture was then filtered
6. customto remove the pyridine hydrochloride
7. washthe filtrate was washed several times with 1N hydrochloric acid solution
8. customThe organic layer was separated
9. customthe solvent was removed by evaporation under reduced pressure
10. customto provide a yellow gum
11. customThe gum was crystallized from ethanol and water