反应详情

2.7 mL 1-bromo-3-chloropropane was added to a mixture of 2 mL thiophen-2-thiol, 5.86 g potassium carbonate and 40 mL N,N-dimethylformamide under ice-cooling and then stirred at room temperature for 2 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated, washed with water plus brine (×2) and then with brine and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was evaporated. The resulting residue was purified by silica gel column chromatography (hexane) to give 4.19 g of the title compound as a pale yellow oil.

1. temperaturecooling
2. customthe organic layer was separated
3. washwashed with water plus brine (×2)
4. dry with materialwith brine and dried over anhydrous sodium sulfate
5. filtrationThe drying agent was filtered off
6. customthe filtrate was evaporated
7. customThe resulting residue was purified by silica gel column chromatography (hexane)