HRID1041123

反应详情

EQUATION

反应方程式

HRID 1041123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a suspension of 5-Chloro-N,N-dimethyl-2-nitro-benzenesulfonamide (1.8 g, 0.0068 mol) and Potassium carbonate (3.3 g, 0.024 mol) in N,N-Dimethylformamide (20 mL, 0.2 mol) was added Dimethylamine hydrochloride (0.83 g, 0.010 mol). The suspension was heated at 50° C. The mixture was cooled to room temperature and poured into water. The precipitate was filtered and rinsed with water then hexane. The recovered material was purified by silica gel chromatography using 0%→20% Methanol:Dichloromethane solvent gradient. 5-Dimethylamino-N,N-dimethyl-2-nitro-benzenesulfonamide isolated as a yellow solid (0.55 g, 30%).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationThe precipitate was filtered
  3. washrinsed with water
  4. customThe recovered material was purified by silica gel chromatography