反应详情

4'-Benzyloxy-3'-(2-benzyloxyethyl)acetophenone (8.0 g) and 30% hydrogen bromide acetic acid solution (0.4 ml) were dissolved in chloroform (80 ml), and a solution of bromine (1.1 ml) in chloroform (30 ml) was added dropwise to the solution over 2 hours at room temperature with stirring, then the resulting mixture was concentrated in vacuo. Purification of the residue by medium pressure liquid column chromatography on silica gel (eluent: hexane/diethyl ether=2/1) gave 4'-benzyloxy-3'-(2-benzyloxyethyl)-2-bromoacetophenone (3.9 g) having a melting point of 53-56° C.

1. concentrationthe resulting mixture was concentrated in vacuo
2. customPurification of the residue by medium pressure liquid column chromatography on silica gel (eluent: hexane/diethyl ether=2/1)