反应详情

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.61 g (7.5 mmol) of 4-(4-(4-chlorobutyl)phenyl)-2-aminothiazole hydrobromide, 2.0 g (7.5 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 2.62 ml (15.0 mmol) of diisopropylethylamine, 1.59 g (15.0 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 3.5 days, cooled, and the precipitate filtered, and the filtrate evaporated. The residue was chromatographed on silica gel using methylene chloride/ethyl acetate and ethyl acetate as eluents. The product fractions were concentrated, taken up in methylene chloride/methanol, precipitated by addition of ethyl acetate saturated with hydrochloride, evaporated, and the residue triturated with ether/ethyl acetate to afford a white solid, m.p. 174°-179° C., 0.87 g (23%).

1. customTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
2. temperatureThe reaction was heated
3. temperatureat reflux for 3.5 days
4. temperaturecooled
5. filtrationthe precipitate filtered
6. customthe filtrate evaporated
7. customThe residue was chromatographed on silica gel
8. concentrationThe product fractions were concentrated
9. customprecipitated by addition of ethyl acetate saturated with hydrochloride
10. customevaporated
11. customthe residue triturated with ether/ethyl acetate
12. customto afford a white solid, m.p. 174°-179° C., 0.87 g (23%)