反应详情

2-(Azetidin-3-yl)-5-chloro-1H-benzo[d]imidazole dihydrochloride, as prepared in preparation 5, (0.16 g, 0.57 mmol) was added to a solution of 2,4,5-trichloropyrimidine (0.11 g, 0.57 mmol) and triethylamine (0.28 mL, 2.00 mmol) in dioxane (2 mL) under argon. The mixture was stirred for 2 h at RT, then dichloromethane and water were added. The resulting layers were separated and the aqueous layer was extracted with dichloromethane. The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to give an oil that was purified by silica gel chromatography to give 5-chloro-2-(1-(2,5-dichloropyrimidin-4-yl)azetidin-3-yl)-1H-benzo[d]imidazole (0.18 g, 0.51 mmol, 89% yield) as a white solid.

1. customThe resulting layers were separated
2. extractionthe aqueous layer was extracted with dichloromethane
3. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto give an oil that
7. customwas purified by silica gel chromatography