HRID1367960

反应详情

EQUATION

反应方程式

HRID 1367960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

5.4 g (20 mmol) of 5-bromo-4-chloroisatoic anhydride was suspended in 20 ml of conc. H2SO4 at −10° C. and cooled to −20° C. 2.1 g (21 mmol) of potassium nitrate was dissolved in 6 mL of sulfuric acid and cooled to 0° C., was then added dropwise to the reaction mixture. The reaction mixture was then stirred 10° C. for 15 min and warmed to room temperature overnight. The mixture was poured in to a beaker containing ice. The resulting solid was collected by filtration, washed with cold water and dried to produce 3.2 g (50%) of 5-bromo-4-chloro-3-nitroisatoic anhydride. LCMS: 323 (M+1)+.

WORKUP

后处理

  1. temperaturecooled to 0° C.
  2. additionwas then added dropwise to the reaction mixture
  3. temperaturewarmed to room temperature overnight
  4. additionThe mixture was poured in to a beaker
  5. additioncontaining ice
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with cold water
  8. customdried