HRID267250

反应详情

EQUATION

反应方程式

HRID 267250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In the same apparatus as in Example 1, 10.0 g of 1,4-naphthoquinone was added to 40 g of fuming sulfuric acid of a sulfur trioxide content of 20 percent maintained at 0° to 5°C, then added thereto 30 g of a mixed acid consisting of 70 percent by weight of sulfuric acid, 25 percent by weight of nitric acid and 5 percent by weight of water dropwise over 1 hour while maintaining the reaction temperature at 15° to 20°C. The reaction mixture was maintained at 15° to 20°C for additional 3 hours and then processed in the same manner as in Example 6 to obtain 11.0 g of crude 5-nitro-1,4-naphthoquinone of a melting point of 153°C. The crude product was purified in the same manner as in Example 6 to obtain the same result as in Example 1.

WORKUP

后处理

  1. temperaturemaintained at 0° to 5°C
  2. additionadded
  3. temperaturewhile maintaining the reaction temperature at 15° to 20°C
  4. temperatureThe reaction mixture was maintained at 15° to 20°C for additional 3 hours