HRID842723

反应详情

EQUATION

反应方程式

HRID 842723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 500 ml round bottom flask fitted with a 250 ml addition funnel and a magnetic stir bar were placed 2,3-ethylenedioxybenzaldehyde (4.07 g, 24.7 mmol) and 100 ml of water. The mixture was heated to 80° and potassium permanganate (7.84 g, 49.6 mmol) in 150 ml of water was added dropwise via the addition funnel over 20 minutes. After the addition was complete the mixture was allowed to stir at 80° for 1.5 hours. The mixture was made basic with a 10% potassium hydroxide solution and the solids filtered. The filter cake was washed with hot water. The filtrate was extracted with ether, made acidic, then extracted with ethyl acetate. The organics were dried over sodium sulfate, filtered, and concentrated to give 2.96 g of subtitled product (66%) which was used directly in the next step.

WORKUP

后处理

  1. customInto a 500 ml round bottom flask fitted with a 250 ml addition funnel and a magnetic stir bar
  2. temperatureThe mixture was heated to 80°
  3. additionAfter the addition
  4. filtrationthe solids filtered
  5. washThe filter cake was washed with hot water
  6. extractionThe filtrate was extracted with ether
  7. extractionextracted with ethyl acetate
  8. dry with materialThe organics were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated