HRID1673144
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
- 60 °C
PROCEDURE
实验过程
To a solution of 2-amino-3-nitrobenzamide (4.0 g, 22 mmol) in warm acetonitrile (1250 mL) was added N-chlorosuccinimide (3.1 g, 23 mmol) and the mixture stirred at 60° C. for 20 hours. After cooling, the orange crystalline material was collected by filtration, washed with acetonitrile and dried. The filtrate was concentrated and the solid recrystallized from acetonitrile to provide a second crop of the title compound. (3.98 g, 84%). MS (DCI/NH3) m/z 216 (M+H)+.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe orange crystalline material was collected by filtration
- washwashed with acetonitrile
- customdried
- concentrationThe filtrate was concentrated
- customthe solid recrystallized from acetonitrile