反应详情

温度

-78 °C

To a 50 mL round-bottomed flask was added 1,4-dibromobenzene (2.85 g, 12.07 mmol) in tetrahydrofuran (40.2 ml). The solution was cooled to −78° C. and n-butyl lithium (4.51 ml, 11.26 mmol) was added dropwise. The mixture was stirred for 1 hour at −78° C. 2-methyl-N-(oxetan-3-ylidene)propane-2-sulfinamide (1.41 g, 8.05 mmol) was added as a tetrahydrofuran solution (ca 1 ml) and the reaction was stirred for 10 minutes and warmed to room temperature. Saturated ammonium chloride was added followed by water and dichloromethane. The aqueous layer was extracted twice with dichloromethane and the combined organics were dried with magnesium sulfate, filtered and concentrated under vacuum. The residue was purified by regular phase, flash column chromatography to give the title compound.

1. stirringthe reaction was stirred for 10 minutes
2. temperaturewarmed to room temperature
3. extractionThe aqueous layer was extracted twice with dichloromethane
4. dry with materialthe combined organics were dried with magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue was purified by regular phase, flash column chromatography