反应详情

温度

120 °C

3-chloropropyltrimethylsilane (33.14 g, 0.22 mol) was added dropwise over 10 minutes to a mixture of 4-hydroxybenzaldehyde (24.4 g, 0.2 mol) and potassium carbonate (30.4 g, 0.22 mol) in 150 ml of dry DMF maintained at 120° C. under nitrogen. The mixture was maintained for 2 hours, 30 minutes, at 120°-130° C. The reaction mixture was cooled and poured into ice-cold water. The aqueous phase was extracted 3 times with dichloromethane. The organic phases were dried over sodium sulfate and concentrated under vacuum. After distillation under vacuum (0.2 mmHg), 40.5 g (yield: 86%) of 4-(3-trimethylsilanylpropyloxy) benzaldehyde were obtained in the form of a colorless oil distilling at 110-114° C. and employed without further purification in the following step.

1. temperatureThe mixture was maintained for 2 hours, 30 minutes, at 120°-130° C
2. temperatureThe reaction mixture was cooled
3. additionpoured into ice-cold water
4. extractionThe aqueous phase was extracted 3 times with dichloromethane
5. dry with materialThe organic phases were dried over sodium sulfate
6. concentrationconcentrated under vacuum
7. distillationAfter distillation under vacuum (0.2 mmHg)