In a 50 mL round-bottom
flask, compound4 (0.15 g; 0.25 mmol) was dissolved in
30 mL of dichloromethane. N-Bromosuccinimide (0.2
g; 0.64 mmol) was dissolved in 10 mL of DCM and added to the reaction
mixture dropwise. After the addition, the reaction mixture was stirred
at room temperature for 3 h. The reaction mixture was extracted with
water (200 mL, three times) and the organic layer was dried over anhydrous
Na2SO4 and concentrated on a rotary evaporator
until the solvent was removed. Compound5 was isolated
from column chromatography on silica gel (230–400 mesh) with
dichloromethane as the eluent (yield: 64%).
flask, compound
30 mL of dichloromethane. N-Bromosuccinimide (0.2
g; 0.64 mmol) was dissolved in 10 mL of DCM and added to the reaction
mixture dropwise. After the addition, the reaction mixture was stirred
at room temperature for 3 h. The reaction mixture was extracted with
water (200 mL, three times) and the organic layer was dried over anhydrous
Na2SO4 and concentrated on a rotary evaporator
until the solvent was removed. Compound
from column chromatography on silica gel (230–400 mesh) with
dichloromethane as the eluent (yield: 64%).
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