反应详情

温度

-25 °C

To a solution of 2-(6,6,6-trifluorohexyl)thiophene (3.33 g) in dry tetrahydrofuran (30 ml) at -25° C. under nitrogen, was added n-butyllithium (8.2 ml, 2.5M) dropwise and the solution stirred at -25° C. for 2 hours. Dry dimethylformamide (2.34 ml) was then added dropwise and the solution stirred for a further hour, allowed to warm to room temperature and stirred for half hour. The reaction mixture was poured onto 2N hydrochloric acid (100 ml), extracted with ether (2×100 ml), dried over MgSO4 and evaporated under reduced pressure to give a brown oil. The oil was distilled under reduced pressure to give a yellow oil b.p. 114° C./1 mm.

1. stirringthe solution stirred for a further hour
2. temperatureto warm to room temperature
3. stirringstirred for half hour
4. extractionextracted with ether (2×100 ml)
5. dry with materialdried over MgSO4
6. customevaporated under reduced pressure
7. customto give a brown oil
8. distillationThe oil was distilled under reduced pressure