反应详情

To a solution of 2-[N-(2-hydroxyethyl)-N-methylamino]pyridine (3.87 g) in dry N,N-dimethylformamide (39 ml) was added sodium hydride (60% in oil, 1.12 g), and the reaction mixture was stirred at room temperature for 30 min. 2-Chloro-4-fluorobenzaldehyde (4.43 g) was added to the reaction mixture and the mixture was stirred for 3 days. The mixture was diluted with ethyl acetate and washed with water. The aqueous layer was extracted twice with ethyl acetate. The organic layers were combined, dried over magnesium sulfate and concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=9/1) to give the objective compound (3.30 g) as a pale-yellow oil.

1. stirringthe mixture was stirred for 3 days
2. washwashed with water
3. extractionThe aqueous layer was extracted twice with ethyl acetate
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated to dryness under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=9/1)