反应详情

温度

50 °C

A solution of 4-thiophen-2-yl-butan-1-ol (4.55 g, 29.09 mmol) in 20 ml of THF was carefully added to a stirred suspension of oil-free sodium hydride (1.05 g, 43.75 mmol) in 15 ml of THF. When the addition was complete, the mixture was heated to 50° C. and stirring continued for 1 hour. Iodomethane (2.7 ml, 43.75 mmol) was then added and the turbid solution was stirred at 50° C. for another 2 hours. After cooling, a few drops of water were added and the mixture was partitioned between 1N-HCl and ether. The organic layer was washed with saturated sodium bicarbonate solution and brine. Drying over sodium sulfate and careful evaporation (product is volatile) gave a pale yellow oil. Yield: 4.45 g (90%).

1. additionWhen the addition
2. stirringthe turbid solution was stirred at 50° C. for another 2 hours
3. temperatureAfter cooling
4. customthe mixture was partitioned between 1N-HCl and ether
5. washThe organic layer was washed with saturated sodium bicarbonate solution and brine
6. dry with materialDrying over sodium sulfate and careful evaporation (product is volatile)
7. customgave a pale yellow oil