反应详情

To a solution of Example 248A (10.0 g, 0.045 mol) in ethanol (100 mL) were added thiourea (3.8 g, 0.05 mol) and triethylamine (6.3 mL, 0.045 mol). The reaction mixture was heated at reflux overnight, then cooled, and concentrated under reduced pressure. The residue was diluted with water (25 mL) and extracted with ethyl acetate (3×50 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography (SiO2, 0-5% methanol in CH2Cl2) to afford the title compound MS (ESI+) m/z 199 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. temperaturecooled
4. concentrationconcentrated under reduced pressure
5. additionThe residue was diluted with water (25 mL)
6. extractionextracted with ethyl acetate (3×50 mL)
7. dry with materialThe combined organic extracts were dried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was purified by column chromatography (SiO2, 0-5% methanol in CH2Cl2)