反应详情

The 5-bromo-2 tetralone (2.0 g, 8.9 mmol), tetrakis(triphenylphosphine)palladium (0.62 g, 0.53 mmol) and zinc cyanide (0.73 g, 6.2 mmol) were added to 4 ml DMF in a 20 ml microwave tube. The mixture was degassed and microwaved at 80° C. for 30 mins. TLC showed no starting material left and the mixture was diluted with ethyl acetate and washed with ammonium hydroxide (2M, ×4 ml). The organic layer was separated and dried over Na2SO4 then filtered. The solvent was evaporated under reduced pressure. The residue was chromatographed through 40 gm Isco Redi-sep column and eluted with 0-30% ethyl acetate-hexane to yield 6-oxo-5,6,7,8-tetrahydronaphthalene-2-carbonitrile.

1. customThe mixture was degassed
2. custommicrowaved at 80° C. for 30 mins
3. waitleft
4. additionthe mixture was diluted with ethyl acetate
5. washwashed with ammonium hydroxide (2M, ×4 ml)
6. customThe organic layer was separated
7. dry with materialdried over Na2SO4
8. filtrationthen filtered
9. customThe solvent was evaporated under reduced pressure
10. customThe residue was chromatographed through 40 gm Isco Redi-sep column
11. washeluted with 0-30% ethyl acetate-hexane