HRID4883

反应详情

EQUATION

反应方程式

HRID 4883 的结构方程式

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

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%).

WORKUP

后处理

  1. customthe flask was purged with nitrogen
  2. additionMethanesulfonic acid (150 mL) was added
  3. additionThe solution was added dropwise to 1 L
  4. temperatureice-cooled water
  5. additionwith the simultaneous addition of 50% aq sodium hydroxide
  6. temperatureto maintain the pH at 2.25 +/-0.25
  7. customThe product was collected by centrifugation
  8. washwashed with water (3×) and acetone (2×)
  9. customThe solid was air-dried
  10. customvacuum-dried at 110° C.