反应详情

温度

35 °C

To a solution of 5-(3-amino-phenyl)-1,1-dioxo-[1,2,5]thiadiazolidin-3-one (5 g, 22 mmol) in 37.5 mL of 9:1 v/v acetonitrile-water was added NaHCO3 (4.62 g, 55 mmol). The mixture was stirred at 25° C. while 2-bromo-1-(2,4-dichloro-phenyl)-ethanone (7.1 g, 26.4 mmol) was added. The mixture was stirred for 12-16 hours at 35° C. The mixture was cooled on an ice bath to further precipitate the product, which was then collected by filtration. The filtrate was concentrated under reduced pressure and a second crop of crude product was collected. The combined crude product was washed once with 25 mL water and dried, then washed once with 10 mL methyl tert-butyl ether and dried, to provide 6.36 g (70% yield) of 5-{3-[2-(2,4-dichloro-phenyl)-2-oxo-ethylamino]-phenyl}-1,1-dioxo-[1,2,5]thiadiazolidin-3-one.

1. additionwas added
2. temperatureThe mixture was cooled on an ice bath
3. customto further precipitate the product, which
4. filtrationwas then collected by filtration
5. concentrationThe filtrate was concentrated under reduced pressure
6. customa second crop of crude product was collected
7. washwas washed once with 25 mL water
8. customdried
9. washwashed once with 10 mL methyl tert-butyl ether
10. customdried