HRID1180682

反应详情

EQUATION

反应方程式

HRID 1180682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Referring to Scheme 5, 237 ml sulfuric acid (concentrate) was first added to a 1 L three-necked flask. 35 g 1,10-phenanthroline was then added into the flask, and the temperature of mixture was kept lower than 100° C. Next, 2436 ml (67%) HNO3 was added drop by drop, and the temperature of mixture was kept lower than 110° C. The mixture was subsequently heated to 100° C. and stirred overnight. After completion of reaction, the reaction mixture was cooled to room temperature and placed into 2 L water, and then NaOH(aq) was added to adjust pH value to a range from 6 to 7, so as to give solids. The solids were washed by water, and dried to obtain solids 5-nitro-1,10-phenanthroline 30 g (0.13 mol, yield 68%).

WORKUP

后处理

  1. additionwas first added to a 1 L three-necked flask
  2. customwas kept lower than 100° C
  3. customwas kept lower than 110° C
  4. customAfter completion of reaction
  5. temperaturethe reaction mixture was cooled to room temperature
  6. customso as to give solids
  7. washThe solids were washed by water
  8. customdried