HRID2248106

反应详情

EQUATION

反应方程式

HRID 2248106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 70% (conc.) nitric acid (20 ml) and glacial acetic acid (10 ml) cooled at 12° C. was treated by drops with 5 g (33.3 mmole) of the compound of Example 3A at a rate to maintain the temperature at 15°-20° C. Stirring was continued for 15 minutes after addition, then the brown slurry was diluted to 100 ml with water and filtered. The solid was washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to 5.40 g (83%) of pure yellow mononitro title compound.

WORKUP

后处理

  1. temperatureto maintain the temperature at 15°-20° C
  2. additionafter addition
  3. filtrationfiltered
  4. washThe solid was washed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated to 5.40 g (83%) of pure yellow mononitro title compound