反应详情

Into a 5 L 3-neck flask equipped with a condenser and a Dean-Stark trap add 3-fluoro-4-triisopropylsilanyloxybenzaldehyde (Example 737, Part A) (90.14 g, 0.3041 mol), ethylene glycol (188.75 g, 3.041 mol), and p-toluenesulfonic acid (0.58 g, 0.003041 mol) in toluene (3.155 L). Heat to boil and reflux until 130 mL of H2O (lower layer) is collected in the Dean-Stark trap (5 hrs). Cool to room temperature, wash with 10% aqueous potassium carbonate solution (2× 1 L) and brine (2× 1 L), and dry over sodium sulfate. Filter and concentrate to give the crude produce.

1. customInto a 5 L 3-neck flask equipped with a condenser
2. temperatureHeat
3. customis collected in the Dean-Stark trap (5 hrs)
4. washwash with 10% aqueous potassium carbonate solution (2× 1 L) and brine (2× 1 L)
5. dry with materialdry over sodium sulfate
6. filtrationFilter
7. concentrationconcentrate
8. customto give the crude
9. customproduce