反应详情

A mixture of 1.15 g of rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol, 1.14 g (4 mmol) of 3-(4-iodophenyl)pyridine, 0.2 g of triphenylphosphine, 50 mg of cuprous iodide, 1.5 ml of triethylamine and 20 ml of acetonitrile was degassed with argon for 10 minutes. Palladium acetate, 75 mg, was then added and stirring was continued for 3 hours. The reaction mixture was partitioned between methylene chloride and water. The organic layer was dried and evaporated. The residue was crystallized from ethyl acetate and recrystallized from methanol/ethyl acetate to give colorless crystals with m.p. 190°-192° C.

1. customwas degassed with argon for 10 minutes
2. additionPalladium acetate, 75 mg, was then added
3. customThe reaction mixture was partitioned between methylene chloride and water
4. customThe organic layer was dried
5. customevaporated
6. customThe residue was crystallized from ethyl acetate
7. customrecrystallized from methanol/ethyl acetate
8. customto give colorless crystals with m.p. 190°-192° C.