反応 #5579

反応方程式

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

triethylamine

methyl chloroformate

→

desired product

収率 66.9%

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

収率 66.9%

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度cooling
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 20 minutes
3. 3
   洗浄The reaction mixture was washed in turn with aqueous sodium bicarbonate and water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONAfter the solvent was distilled off
6. 6
   その他the residue was purified by column chromatography [eluent: ethanol/etyl acetate (1:10)]

実験手順

To a solution of 5-[2-(amino)ethylthio]imidazo[1,2-a]pyridine (1.93 g, 10 mmoles) and triethylamine (1.53 ml, 11 mmoles) in methylene chloride (30 ml) was added methyl chloroformate (0.77 ml, 10 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 20 minutes. The reaction mixture was washed in turn with aqueous sodium bicarbonate and water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography [eluent: ethanol/etyl acetate (1:10)] to obtain 1.68 g of the desired product (66.9%, colorless crystals).

出典