反应详情

To a stirred solution of 5-bromo-2-methoxybenzaldehyde (5.0 g, 23.25 mmol) in toluene (50 mL) was added ethylene glycol (2.6 mL, 46.5 mmol) and p-toluenesulfonic acid monohydrate (0.45 g, 2.32 mmol) and the reaction mixture was azeotroped for 2 h, quenched with sat. NaHCO3 (50 mL). Reaction mixture was concentrated under reduced pressure, extracted with ethyl acetate (2×100 mL), washed with water, brine, dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 2-(5-bromo-2-methoxy-phenyl)-[1,3]dioxolane (3.75 g).

1. customthe reaction mixture was azeotroped for 2 h
2. customquenched with sat. NaHCO3 (50 mL)
3. customReaction mixture
4. concentrationwas concentrated under reduced pressure
5. extractionextracted with ethyl acetate (2×100 mL)
6. washwashed with water, brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. custompurified by silica gel column chromatography