HRID629676

反应详情

EQUATION

反应方程式

HRID 629676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

2,3-dihydrobenzofuran (5 g, 41.6 mmol) was dissolved in 35 mL of acetic acid, and ¼ HNO3 (0.9 mL, 45.4 mmol) was added dropwise. At the beginning of reaction, it was heated to 70° C., then the residual HNO3 was added. After 0.5 hour, the reaction was cooled, added into ice-water, and then neutralized with Na2CO3. The water layer was extracted with ethyl acetate. The organic layers were combined and dried, concentrated under vacuum, purified by column chromatography to obtain a product (1 g, 14.6%).

WORKUP

后处理

  1. customAt the beginning of reaction, it
  2. temperaturethe reaction was cooled
  3. extractionThe water layer was extracted with ethyl acetate
  4. customdried
  5. concentrationconcentrated under vacuum
  6. custompurified by column chromatography