反应详情

温度

65 °C

Resorcinol (33.0 g, 0.300 mol) and succinic anhydride (30.0 g, 0.300 mol) were placed in a round bottomed flask and purged with nitrogen. Methanesulfonic acid (150 mL) was added and the solution was stirred at 65° C. for 2 hours under an atmosphere of nitrogen. The reaction mixture was added dropwise to rapidly stirred, ice-cooled water (1 L) with simultaneous addition of 50% aqueous sodium hydroxide to maintain pH 2.5 +/0.5. The product which appeared as a granular precipitate was collected by filtration and rinsed with water (3×100 mL) then acetone (3×100 mL). The product was air-dried then vacuum-dried (vacuum oven) at 110° C. for 18 hours to afford a dark red powder (37.7 g, 88%).

1. custompurged with nitrogen
2. additionMethanesulfonic acid (150 mL) was added
3. additionThe reaction mixture was added dropwise
4. stirringto rapidly stirred
5. temperatureice-cooled water (1 L)
6. additionwith simultaneous addition of 50% aqueous sodium hydroxide
7. temperatureto maintain pH 2.5 +/0.5
8. filtrationwas collected by filtration
9. washrinsed with water (3×100 mL)
10. customThe product was air-dried
11. customthen vacuum-dried (vacuum oven) at 110° C. for 18 hours