反应 #6180

反应方程式

Triethylamine

2-mercaptopyridine

N-(2-bromoethyl)phthalimide

→

desired compound

收率 46.9%

2-(2-phthalimidoethylthio)pyridine

收率 46.9%

溶剂

ethanol

反应条件

后处理

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
   洗涤the mixture was washed with water
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   其他the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane=1:2)

实验过程

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).

来源