HRID1532591
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto cool to room temperature
- additionwas poured into a flask
- customThe yellow solid was collected
- dissolutionwas dissolved in dichloromethane (1.5 L)
- customresulting in two-phases
- customThe organic layer was collected
- dry with materialwas dried over magnesium sulfate
- filtrationfiltered
- customthe solvents were removed under reduced pressure by rotary evaporation