反应详情

温度

0 °C

To a solution of compound 8C (0.80 g, 4.15 mmol) in chloroform (2.4 mL) cooled to −20° C. was slowly added a solution of bromine (0.22 mL, 4.35 mmol) in chloroform (1 mL) so that the reaction temperature was maintained below −10° C. The reaction was stirred at 0° C. for 5 min, and then quenched immediately with water. The mixture was extracted with CH2Cl2 (3×), the combined extracts washed with saturated NaHCO3, brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with CH2Cl2 to afford the title compound (0.98 g).

1. temperaturewas maintained below −10° C
2. customquenched immediately with water
3. extractionThe mixture was extracted with CH2Cl2 (3×)
4. washthe combined extracts washed with saturated NaHCO3, brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was chromatographed (silica gel)
9. washeluting with CH2Cl2