反应 #4979

反应方程式

4-Methylresorcinol

succinic anhydride

→

powder

收率 74.2%

9-Carboxyethylidene-3,6-dihydroxy-2,7-dimethyl-9H-xanthene

收率 74.2%

反应条件

后处理

1. 1
   其他the flask was purged with nitrogen
2. 2
   workup.ADDITIONMethanesulfonic acid (150 mL) was added
3. 3
   workup.ADDITIONThe solution was added dropwise to 1 L
4. 4
   温度ice-cooled water
5. 5
   workup.ADDITIONwith the simultaneous addition of 50% aq sodium hydroxide
6. 6
   温度to maintain the pH at 2.25 +/-0.25
7. 7
   其他The product was collected by centrifugation
8. 8
   洗涤washed with water (3×) and acetone (2×)
9. 9
   其他The solid was air-dried
10. 10
    其他vacuum-dried at 110° C.

实验过程

4-Methylresorcinol (25.8 g, 0.208 mol) and succinic anhydride (20.8 g, 0.208 g) were placed in a round bottom flask and the flask was purged with nitrogen. Methanesulfonic acid (150 mL) was added and the solution heated under nitrogen to 65° C. for 2 hours. The solution was added dropwise to 1 L of rapidly stirred, ice-cooled water with the simultaneous addition of 50% aq sodium hydroxide to maintain the pH at 2.25 +/-0.25. The product was collected by centrifugation and washed with water (3×) and acetone (2×). The solid was air-dried, then vacuum-dried at 110° C. to afford a brick-red powder (24.1 g, 74%).

来源