反应详情

A solution of 4-chloro-5-[4-chloro-2-(trifluoromethyl)phenyl]benzene-1,2-diamine (100 mg, 0.31 mmol, 1.00 equiv) in heptafluorobutanoic acid (5 ml) was stirred overnight at 80° C. in an oil bath and then quenched with ice-water (30 ml). The pH value of the solution was adjusted to 8 with saturated aqueous sodium carbonate and extracted with ethyl acetate (50 ml×3). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under vacuum to give a residue, which was purified by Pre-TLC with 10% ethyl acetate in petroleum ether to produce 5-chloro-6-[4-chloro-2-(trifluoromethyl)phenyl]-2-(heptafluoropropyl)-1H-1,3-benzodiazole as a off-white solid (105.8 mg, 68%).

1. customquenched with ice-water (30 ml)
2. extractionextracted with ethyl acetate (50 ml×3)
3. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
4. concentrationconcentrated under vacuum
5. customto give a residue, which
6. customwas purified by Pre-TLC with 10% ethyl acetate in petroleum ether