反応 #168852

反応方程式

triethylamine

N,N,N′-trimethylethane-1,2-diamine

tetrahydrofuran

5,6-dichloropyridine-3-sulfonyl chloride

→

5,6-dichloro-N-[2-(dimethylamino)ethyl]-N-methylpyridine-3-sulfonamide

収率 73.0%

溶媒

water

反応条件

後処理

1. 1
   その他obtained in the above reaction
2. 2
   抽出extracted with chloroform
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=5:1 to 3:1)

実験手順

With cooling with ice, triethylamine (0.57 ml, 4.06 mmol) and N,N,N′-trimethylethane-1,2-diamine (0.30 ml, 2.23 mmol) were added to a tetrahydrofuran solution (5 ml) of 5,6-dichloropyridine-3-sulfonyl chloride (500 mg, 2.03 mmol) obtained in the above reaction, and stirred for 5 minutes. Saturated saline water was added to the reaction solution, extracted with chloroform, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=5:1 to 3:1) to obtain 5,6-dichloro-N-[2-(dimethylamino)ethyl]-N-methylpyridine-3-sulfonamide (460 mg, yield: 73%) as a red solid.

出典