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温度

0 °C

2,4-dichlorobenzaldehyde (26.26 g, 0.15 mol) was dissolved in toluene (200 mL), and then KOH (8.4 g, 1 eq) in water (183 mL) was added followed by BnEt3NCl. The mixture was cooled to 0° C. and n-propanal (26.15 g, 0.45 mol, 3 eq) in toluene (50 mL) was added dropwise. The mixture was allowed to warm to room temperature and stirred overnight. The organic layer was separated and washed successively with water, brine, dried (MgSO4), and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (0-1-2-3% EtOAc in hexanes) to give 17.56 g of 3-(2,4-dichlorophenyl)-2-methylpropenal.

1. temperatureto warm to room temperature
2. customThe organic layer was separated
3. washwashed successively with water, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by silica gel chromatography (0-1-2-3% EtOAc in hexanes)