反応 #6286

反応方程式

4-mercaptopyridine

1-bromo-4-chlorobutane

triethylamine

→

desired compound

収率 89.7%

4-(4-chlorobutylthio)pyridine

収率 89.7%

溶媒

ethanol

反応条件

後処理

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

実験手順

To a suspension of 33.35 g (0.30 mol) of 4-mercaptopyridine and 51.44 g (0.30 mol) of 1-bromo-4-chlorobutane in 500 ml of ethanol, 41.9 ml (0.30 mol) of triethylamine was added, and the mixture was stirred at room temperature for 5 hours. The solvent was distilled off and chloroform was added to the residue. 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 =1:1) to give 54.27 g of the desired compound (89.7% yield, colorless oil).

出典