反应详情

2-Chloro-N-(4-chlorophenyl)-3-oxobutanamide (24.7 g, 0.1 mole), 1,2-ethanedithiol (9.4 g, 0.1 mole) and a small amount of p-toluenesulfonic acid were heated under reflux in benzene (150 ml), using a Dean-Stark trap to remove water (1.9 ml collected). The reaction mixture was filtered, treated with triethylamine (8 ml), and refluxed for a further 30 minutes. The mixture was then washed with water, dilute hydrochloric acid, and water. Evaporation of the benzene gave a white solid, which was recrystallized from absolute ethanol. The product melted at 115°-117° C. (24 g, 84% yield).

1. customto remove water (1.9 ml collected)
2. filtrationThe reaction mixture was filtered
3. additiontreated with triethylamine (8 ml)
4. temperaturerefluxed for a further 30 minutes
5. washThe mixture was then washed with water, dilute hydrochloric acid, and water
6. customEvaporation of the benzene
7. customgave a white solid, which
8. customwas recrystallized from absolute ethanol