反应详情

温度

110 °C

In the solution of 220 g(2 mol) of catechol in 500 ml of acetic acid, 102 g(1 mol) of acetic anhydride was drop-added for one hour while agitating the solution at 110° C. The mixture was maintained at 110° C. for two hours, and diethylene glycol dibutyl ether was distilled under vacuum. 1 Liter of toluene was added to the reaction mixture and cooled to 0° C. and then the unreacted excess hydroquinone was filtered and collected (recovered amount: 110 g, recycled without any purification process). A desired mono acetyl catechol was obtained by evaporating the residue in vacuum. (Yield: 149.0 g(98%). mp: oil. 1H-NMR(200 MHz, CDCl3, ppm) 2.33(s, 3H), 5.81 (br, 1H), 6.83-7.18 (m, 4H).

1. temperatureThe mixture was maintained at 110° C. for two hours
2. distillationdiethylene glycol dibutyl ether was distilled under vacuum
3. addition1 Liter of toluene was added to the reaction mixture
4. temperaturecooled to 0° C.
5. filtrationthe unreacted excess hydroquinone was filtered
6. customcollected (
7. customrecovered amount