反应详情

4-Bromo-3-fluorobenzaldehyde (100.00 g, 492.6 mmol) was added to toluene (1 L). Propane-1,3-diol (42.72 mL, 591.1 mmol), and p-toluenesulfonic acid monohydrate (4.685 g, 24.63 mmol) were added to above and the reaction mixture was brought to reflux. The solvent (500 mL) was azeotroped off using a dean stark trap. The reaction mixture was cooled and extracted with sat. aqueous sodium bicarbonate (500 mL). The organics were dried over magnesium sulfate and concentrated in vacuo to give 2-(4-bromo-3-fluorophenyl)-1,3-dioxane as a white solid. MS (ESI) m/z: Calculated: 260.0/262.0; Observed: 260.9 (M++1).

1. temperatureto reflux
2. customThe solvent (500 mL) was azeotroped off
3. temperatureThe reaction mixture was cooled
4. extractionextracted with sat. aqueous sodium bicarbonate (500 mL)
5. dry with materialThe organics were dried over magnesium sulfate
6. concentrationconcentrated in vacuo