反応 #6180

反応方程式

Triethylamine

2-mercaptopyridine

N-(2-bromoethyl)phthalimide

→

desired compound

収率 46.9%

2-(2-phthalimidoethylthio)pyridine

収率 46.9%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度under reflux for 2 hours
3. 3
   workup.DISTILLATIONThe solvent was distilled off
4. 4
   workup.ADDITIONchloroform was added to the residue
5. 5
   洗浄the mixture was washed with water
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   その他the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:2)

実験手順

Triethylamine [12.54 ml (90 mmol)] was added to a suspension of 6.67 g (60 mmol) of 2-mercaptopyridine and 15.24 g (60 mmol) of N-(2-bromoethyl)phthalimide in 200 ml of ethanol and stirred at room temperature for 24 hours. The mixture was heated under reflux for 2 hours. The solvent was distilled off, chloroform was added to the residue, and the mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:2) to obtain 8.00 g of the desired compound (46.9%, colorless crystals).

出典