Boron tribromide → HCID 71626584, compound

Participants

Reaction Steps

Dissolve compound 6 (6 g, 0.0201 mol) in 50 ml dichloromethane, add drop wise BBr3 solution in methylene chloride (24 ml, 1M) at 0° C., react at room temperature for 1 h. Wash the reaction solution with water, dry over anhydrous magnesium sulfate. Filter the solution and remove the solvent by rotary evaporation, dissolve the residue with petroleum ether/diethyl ether and feed the solution to a silica gel column, evaporate the solvent in eluent to obtain 5.4 g white solid (95%). 1H-NMR (400M, CDCl3) δ (ppm): 3.79 (s, 3H), 3.82 (s, 3H), 6.40 (d, J=2.4 Hz, 1H), 6.80 (d, J=2.4 Hz, 1H), 7.15 (dd, J=16 Hz, 2H), 7.28 (t, J=7.2 Hz, 1H), 7.38 (t, J=7.2 Hz, 2H), 7.52 (d, J=7.2 Hz, 2H), 10.28 (s, 1H).

Provenance & Evidence