反应详情

温度

-78 °C

6-Bromo-2,2-dimethyl-2H-chromene (10 mmoL) in THF (20 mL) was treated with n-butyl lithium (15 mmoL) dropwise at −78° C. The resulting solution was stirred at −78° C. for 30 min. Benzene disulfide (10 mmoL) in THF (10 mL) was then added dropwise into the reaction over about 15 min. The reaction mixture was kept at −78° C. and slowly warmed to room temperature over 2 hrs. The solvent was removed and the residue was partitioned between diethyl ether and water. The combined organic layer was washed with brine, filtered, dried over anhydrous Na2SO4 and concentrated to yield crude material, which was purified by silica gel chromatography to yield the title compound as a white solid.

1. customwas kept at −78° C.
2. temperatureslowly warmed to room temperature over 2 hrs
3. customThe solvent was removed
4. customthe residue was partitioned between diethyl ether and water
5. washThe combined organic layer was washed with brine
6. filtrationfiltered
7. dry with materialdried over anhydrous Na2SO4
8. concentrationconcentrated
9. customto yield crude material, which
10. customwas purified by silica gel chromatography