HRID1893558

反应详情

EQUATION

反应方程式

HRID 1893558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-Methoxy-1-tetralone (12.0 g, 68.1 mmol) was dissolved in acetic anhydride (60 ml), a fuming nitric acid (4.8 ml)-acetic acid (4.2 ml) mixed solvent was slowly added dropwise under ice-cooling with stirring, and thereafter the mixture was stirred at the same temperature for 2 hr. The reaction mixture was diluted with ether, and the precipitated solid was collected by filtration and dried under reduced pressure. The obtained solid was recrystallized from benzene (100 ml), and the precipitated solid was filtered, dried under reduced pressure to give the title compound (3.62 g, yield 24%) as a colorless solid.

WORKUP

后处理

  1. additionwas slowly added dropwise under ice-
  2. temperaturecooling
  3. stirringthe mixture was stirred at the same temperature for 2 hr
  4. filtrationthe precipitated solid was collected by filtration
  5. customdried under reduced pressure
  6. customThe obtained solid was recrystallized from benzene (100 ml)
  7. filtrationthe precipitated solid was filtered
  8. customdried under reduced pressure