反应详情

温度

-78 °C

Combine 3-bromodibenzofuran (0.5 g, 2.0 mmol) and tetrahydrofuran (30 ml). Cool to about −78° C. Add a solution of t-butyllithium, 1.6 M solution in hexane (2.2 ml, 3.0 mmol), then warm to about 0° C. for 10 min. Cool to about −78° C. and add dimethylformamide (0.5 ml, 5.9 mmol). Warm to room temperature, quench with water, and extract with dichloromethane. Combine the organic layers and wash sequentially with distilled water and brine and then dry (Na2SO4), filter, and concentrate to give a residue. Chromatograph the residue eluting with 8:2 hexane:EtOAc to give the title compound.

1. temperaturewarm to about 0° C. for 10 min
2. temperatureCool to about −78° C.
3. temperatureWarm to room temperature
4. customquench with water
5. extractionextract with dichloromethane
6. washwash sequentially with distilled water and brine
7. dry with materialdry (Na2SO4)
8. filtrationfilter
9. concentrationconcentrate
10. customto give a residue
11. washChromatograph the residue eluting with 8:2 hexane