反应详情

温度

80 °C

In a round bottomed flask equipped with magnetic stirring, reflux condenser, N2 atmosphere, and a heating mantle was placed DMF (80 ml) and to this was added cautiously NaH (60% by weight in oil, 1.76 g) followed by 3,4-dichlorophenol (7.15 g). This mixture was stirred for ten minutes then 1-[4-acetamidophenoxy]-3-chloropropane of Formula XXI (10.0 g) was added; and the reaction mixture heated at 80° C. overnight. The mixture was cooled and the DMF removed in vacuo. The residue was poured into ice water and the precipitated brown solid was collected by filtration. The crude product was recrystallized from ethanol to give an off white solid (9.8 g), mp 135°-7° C.

1. customIn a round bottomed flask equipped with magnetic stirring
2. temperaturereflux condenser
3. temperatureThe mixture was cooled
4. customthe DMF removed in vacuo
5. additionThe residue was poured into ice water
6. filtrationthe precipitated brown solid was collected by filtration
7. customThe crude product was recrystallized from ethanol