反应详情

温度

-30 °C

To a solution of 2-(4-chlorophenylthio)thiophene (9.8 g) in dry tetrahydrofuran (75 ml) at -30° C. under nitrogen, was added dropwise, n-butyllithium (17.4 ml, 2.5M) and the solution left to stir at -30° C. for 2 hours. Dry dimethylformamide (5.1 ml) was then added and the solution allowed to stir at -30° C. for a further hour, warmed to room termperature and stirred overnight. The reaction mixture was poured onto 2N hydrochloric acid (75 ml), extracted with ether (2×100 ml), dried over MgSO4 and evaporated under reduced pressure to give a brown oil. The oil was flash chromatographed on a Sorbsil C60-40/60H column using 25% ether-hexane to give an orange oil.

1. stirringto stir at -30° C. for a further hour
2. temperaturewarmed to room termperature
3. stirringstirred overnight
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. customchromatographed on a Sorbsil
9. customto give an orange oil