反応 #48493

反応方程式

3-((6-chloronaphthalen-2-yl)sulfonyl)propinoic acid

HOBt

WSC

1-(piperidin-4-yl)-2-pyrrolidinone

→

title compound

収率 39.0%

1-(1-{3-[(6-Chloronaphthalen-2-yl)sulfonyl]propanoyl}piperidin-4-yl)pyrrolidin-2-one

収率 39.0%

溶媒

DMF

triethylamine

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   その他The organic layer was separated
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他The residue was purified by basic silica gel column chromatography (ethyl acetate to ethyl acetate/methanol 10/1)

実験手順

After 3-((6-chloronaphthalen-2-yl)sulfonyl)propinoic acid (0.30 g), HOBt (0.23 g) and WSC (0.29 g) were dissolved in DMF (10 mL), 1-(piperidin-4-yl)-2-pyrrolidinone (0.17 g) and triethylamine (0.10 g) were added thereto, and the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and diluted with ethyl acetate and an aqueous sodium bicarbonate solution. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate to ethyl acetate/methanol 10/1) to obtain the title compound (0.17 g, 39%) as a colorless powder.

出典