反应详情

温度

80 °C

A suspension of 5-bromo-2-(3-ethylureido)pyridine-4-carbothioamide (Intermediate 6, 160 g, 510 mmol), 3-bromo-1,1,1-trifluoroacetone (200 g, 1.02 mol) in acetonitrile (3 L) was heated at 80° C. for 20 h. The solution was then cooled down and concentrated. 2:1 Acetonitrile: methyl tert-butyl ether (2.4 L) was added, and the solution thus obtained was placed on a rotovap, and the volume of solvent was reduced by half. The precipitate that formed was filtered and dried in a vacuum oven at 40° C. After letting the filtrate sit, more solid precipitated out and an additional two crops of precipitate were collected and dried in the vacuum oven at 40° C. resulting in a combined collection of 202.4 g (92%) of 1-(5-bromo-4-(4-hydroxy-4-(trifluoromethyl)-4,5-dihydrothiazol-2-yl)pyridin-2-yl)-3-ethylurea as pale yellow solid.

1. temperatureThe solution was then cooled down
2. concentrationconcentrated
3. addition2:1 Acetonitrile: methyl tert-butyl ether (2.4 L) was added
4. customthe solution thus obtained
5. customThe precipitate that formed
6. filtrationwas filtered
7. customdried in a vacuum oven at 40° C
8. custommore solid precipitated out
9. customan additional two crops of precipitate were collected
10. customdried in the vacuum oven at 40° C.