反応 #1470251

反応方程式

3-Amino-1-ethylpiperidine

sodium carbonate

4-(7-chloro-4-cinnolinylamino)benzenesulphonylchloride hydrochloride

→

4-[7-Chloro-4-cinnolinylamino]-N-(1-ethyl-3-piperidyl)benzenesulphonamide

title compound

溶媒

chloroform

water

反応条件

後処理

1. 1
   workup.STIRRINGThe dark orange mixture was stirred at 3° C. for 15 minutes
2. 2
   workup.WAITDuring this period the colour lightened considerably
3. 3
   その他The chloroform layer was separated
4. 4
   乾燥dried over magnesium sulphate
5. 5
   その他The residue on evaporation
6. 6
   その他triturated with methanol

実験手順

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).

出典