反应详情

A 500 mL four-necked flask equipped with a reflux condenser, a stirrer, a thermometer, and a nitrogen inlet tube was charged with 28.1 g (0.18 mol) of 1-adamantanol, 15.84 g (0.09 mol) of p-toluenesulfonic acid monohydrate, and 300 mL of heptane and replaced with nitrogen. The mixture was added with 9.9 g (0.09 mol) of resorcinol. The flask was immersed in an oil bath at 100° C. and the mixture was heated while stirring for 1 hour. After cooling the reaction mixture, the solid content was collected by filtration, which was then dried under vacuum, followed by recrystallization by aqueous methanol solution to obtain 4,6-bis(1-adamantyl)-1,3-dihydroxybenzene (yield: 86%, LC (liquid chromatography) purity: 99.7%, melting point: 146° C.). Note that the LC purity was measured by absorbance at λ=280 nm.

1. customA 500 mL four-necked flask equipped with a reflux condenser, a stirrer
2. customThe flask was immersed in an oil bath at 100° C.
3. temperaturethe mixture was heated
4. temperatureAfter cooling the reaction mixture
5. filtrationthe solid content was collected by filtration, which
6. customwas then dried under vacuum
7. customfollowed by recrystallization by aqueous methanol solution