反应详情

A mixture of 4-carboxybenzaldehyde (21.9 g, 145.9 mmol), 3,3,4,4,4-pentafluoro-2-butanol (24.1 g, 146.9 mmol), EDC (33.5 g, 174.8 mmol) and DMAP (18.1 g, 148.1 mmol) was dissolved in DMF (60 ml) at rt. It was stirred for 36 h at rt. Hexane was added, it was washed with 1 N HCl, sat NaHCO3 and brine. The aqueous layers were extracted three times with hexane. It was dried over Na2SO4, filtered, concentrated, and the residue was purified by silica gel chromatography (ethyl acetate:hexane 1:10) to yield the desired aldehyde as a yellow oil (67%).

1. washit was washed with 1 N HCl
2. extractionThe aqueous layers were extracted three times with hexane
3. dry with materialIt was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customthe residue was purified by silica gel chromatography (ethyl acetate:hexane 1:10)