反应详情

To a mixture of the amidine of step 1 (2.0 g, 7.1 mmol) and sodium bicarbonate (1.2 g, 14.3 mmol) in isopropanol (200 ml), 3-bromo-1,1,1-trifluoroacetone 1.1 ml, 10.7 mmol) was added. After heating at 80–85° C. for 16 hours, the reaction mixture was cooled and filtered. The residue was washed with methylene chloride and the combined organic fractions were dried over sodium sulfate, filtered and concentrated. The crude mixture (25.7 g) was purified by chromatography (silica gel, ethyl acetate/hexane 55/45) to give the 4,5-dihydro-imidazole (1.1 g, 38%) as a white solid: mp (DSC) 214° C. Anal. Calcld. for C15H13N2S2O3F3: C, 46.15, H, 3.36, N, 7.18, S, 16.43. Found: C, 46.09, H, 3.26, N, 7.07, S, 16.71.

1. additionwas added
2. temperatureAfter heating at 80–85° C. for 16 hours
3. temperaturethe reaction mixture was cooled
4. filtrationfiltered
5. washThe residue was washed with methylene chloride
6. dry with materialthe combined organic fractions were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude mixture (25.7 g) was purified by chromatography (silica gel, ethyl acetate/hexane 55/45)