反应详情

温度

145 °C

A 500 ml round bottom flask is equipped with a mechanical stirrer, thermometer and condenser. Add 50 grams 1,1,1-tris(4-hydroxyphenyl)ethane, 100 grams DMF, 0.5 g. potassium iodide and 47.4 grams of ethylene carbonate. Heat to 145° C. and hold for 6 hours. Add 200 g. ethyl acetate and wash the organic portion four times with 150 g. saturated brine. Strip the solvent from the mix on a rotary evaporator. The yield of tan solid is 78 grams. Recrystallize this crude product by dissolving in 300 g. boiling ethyl acetate and allowing to cool slowly. Collect 70.3 grams of a tan solid; the mp=78-81° C.

1. customA 500 ml round bottom flask is equipped with a mechanical stirrer
2. additionAdd 200 g
3. washethyl acetate and wash the organic portion four times with 150 g
4. additionStrip the solvent from the mix on a rotary evaporator
5. customRecrystallize this crude product
6. dissolutionby dissolving in 300 g
7. temperatureto cool slowly
8. customCollect 70.3 grams of a tan solid