HRID1532591

反应详情

EQUATION

反应方程式

HRID 1532591 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

4,5-Dichloro-2-nitroaniline (15.2 g, 73.2 mmol), N-chlorosuccinimide (12.2 g, 91.6 mmol) and N,N-dimethylformamide (150 mL) were combined and the resulting orange solution was heated to 100° C. for 1 h. The solution was allowed to cool to room temperature and was poured into a flask containing ice water (1.2 L). The yellow solid was collected and was dissolved in dichloromethane (1.5 L), resulting in two-phases. The organic layer was collected and was dried over magnesium sulfate, filtered and the solvents were removed under reduced pressure by rotary evaporation to leave 17.6 g (98%) of a yellow solid. MS (Cl): m/z 239.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. additionwas poured into a flask
  3. customThe yellow solid was collected
  4. dissolutionwas dissolved in dichloromethane (1.5 L)
  5. customresulting in two-phases
  6. customThe organic layer was collected
  7. dry with materialwas dried over magnesium sulfate
  8. filtrationfiltered
  9. customthe solvents were removed under reduced pressure by rotary evaporation