反応 #166397

反応方程式

6-chloropyridine-3-sulfonyl chloride

tert-butyl 1-piperazinecarboxylate

triethylamine

methanol DCM

→

compound 360

収率 84.7%

tert-Butyl 4-((6-chloro-3-pyridinyl)sulfonyl)-1-piperazinecarboxylate

収率 84.7%

溶媒

DCM

反応条件

後処理

1. 1
   温度gradually warmed up to ambient temperature for 1.5 h

実験手順

To a stirred ice-cooled solution of tert-butyl 1-piperazinecarboxylate (0.88 g, 4.7 mmol), triethylamine (1.3 mL, 9.4 mmol), and 4-dimethylaminopyridine (0.0058 g, 0.047 mmol) in DCM (10 mL) was added 6-chloropyridine-3-sulfonyl chloride (1.0 g, 4.7 mmol) in one portion. The resulting mixture was stirred at 0° C. and gradually warmed up to ambient temperature for 1.5 h. Upon workup, the mixture was directly subjected to combi-flash column chromatography (methanol/DCM) to give compound 360 (1.44 g, 84% yield) as a white solid.

出典