HRID649650

反应详情

EQUATION

反应方程式

HRID 649650 的结构方程式

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

0.103 mol (17.2 g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), the temperature being maintained at between 0° C. and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice; the expected product precipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.). It can optionally be recrystallized from 96° strength ethanol.

WORKUP

后处理

  1. temperaturethe temperature being maintained at between 0° C. and 5° C
  2. addition1 hour after the addition
  3. customthe expected product precipitates
  4. dry with materialAfter being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.)
  5. customIt can optionally be recrystallized from 96° strength ethanol