反应详情

To a solution of N-phenylpiperazine (200 mg) and diiosopropylethylamine (130 mg) in dimethylformamide (1 ml) was added 3-[[(methylsulfonyl)oxy]methyl]-4-phenylmethoxybenzaldehyde (320 mg). After stirring at room temperature for 3 hours the reaction mixture was partially concentrated under reduced pressure and the residue was purified by flash chromatography column using petroleum ether:diethyl ether (1:3) as eluant. The pure fractions were combined and evaporated under reduced pressure to give a gum which was crystallized from diethyl ether to give 4-phenylmethoxy-3-[[(4-phenyl)-1-piperazinyl]methyl]benzaldehyde (320 mg) as white crystals. 1H NMR (CDCl3) δ9.95 (s, 1H, CHO); 5.23 (s, 2H); 3.80 (s, 2H); 3.30 (m, 4H); 2.78 (m, 4H). TLC (silica gel): Rf=0.7 (petroleum ether:diethyl ether, 1:4).

1. concentrationwas partially concentrated under reduced pressure
2. customthe residue was purified by flash chromatography column
3. customevaporated under reduced pressure
4. customto give a gum which
5. customwas crystallized from diethyl ether