반응 #168854

반응 방정식

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

수율 69.0%

용매

water

반응 조건

후처리

1. 1
   추출extracted with chloroform
2. 2
   건조the organic layer was dried over anhydrous sodium sulfate
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=6:1 to 4:1)

실험 절차

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.

출처