HRID235653

反应详情

EQUATION

反应方程式

HRID 235653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
3 °C

PROCEDURE

实验过程

3-Amino-1-ethylpiperidine (0.4 ml) in chloroform (15 ml) was treated with anhydrous sodium carbonate (2.94 g) in water (15 ml) and cooled to 3° C. The mixture was vigorously stirred and treated with 4-(7-chloro-4-cinnolinylamino)benzenesulphonylchloride hydrochloride (1.0 g). The dark orange mixture was stirred at 3° C. for 15 minutes, then at room temperature for 45 minutes. During this period the colour lightened considerably. The chloroform layer was separated and dried over magnesium sulphate. The residue on evaporation solidified when triturated with methanol, to give the title compound (0.5 g), m.p. 213°-15° C. (with decomposition).

WORKUP

后处理

  1. stirringThe dark orange mixture was stirred at 3° C. for 15 minutes
  2. waitDuring this period the colour lightened considerably
  3. customThe chloroform layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customThe residue on evaporation
  6. customtriturated with methanol