反応 #5539

反応方程式

water

5-[2-(amino)ethylthio]imidazo[1,2-a]pyridine dihydrochloride

triethylamine

acetyl chloride

→

desired product

収率 66.8%

5-[2-(acetylamino)ethylthio]imidazo[1,2-a]pyridine

収率 66.8%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度cooling
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 4 hours
3. 3
   抽出extracted with chloroform
4. 4
   洗浄The chloroform layer was washed with saturated saline
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONAfter the solvent was distilled off
7. 7
   その他the residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:3)

実験手順

To a solution of 5-[2-(amino)ethylthio]imidazo[1,2-a]pyridine dihydrochloride (2.66 g, 10 mmoles) and triethylamine (4.32 ml, 31 mmoles) in N,N-dimethylformamide (24 ml) was added acetyl chloride (0.71 ml, 10 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 4 hours. The reaction mixture was poured into water and extracted with chloroform. The chloroform layer was washed with saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:3) to obtain 1.57 g of the desired product (66.8%, colorless crystals).

出典