反応 #168854

反応方程式

triethylamine

N,N,N′-trimethylpropane-1,3-diamine

tetrahydrofuran

5,6-dichloropyridin-3-sulfonyl chloride

→

5,6-dichloro-N-[3-(dimethylamino)propyl]-N-methylpyridine-3-sulfonamide

収率 69.0%

溶媒

water

反応条件

後処理

1. 1
   抽出extracted with chloroform
2. 2
   乾燥the organic layer was dried over anhydrous sodium sulfate
3. 3
   濃縮concentrated under reduced pressure
4. 4
   その他The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=6:1 to 4:1)

実験手順

With cooling with ice, triethylamine (0.57 ml, 4.06 mmol) and N,N,N′-trimethylpropane-1,3-diamine (0.34 ml, 2.23 mmol) were added to a tetrahydrofuran solution (5 ml) of 5,6-dichloropyridin-3-sulfonyl chloride (500 mg, 2.03 mmol), and stirred for 5 minutes. Saturated saline water was added to the reaction solution, extracted with chloroform, and the organic layer was dried over anhydrous sodium sulfate, concentrated under reduced pressure. The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=6:1 to 4:1) to obtain 5,6-dichloro-N-[3-(dimethylamino)propyl]-N-methylpyridine-3-sulfonamide (454 mg, yield: 69%) as a red solid.

出典