反应详情

A mixture of intermediate D15 (0.15 g, 0.418 mmol), intermediate D4 (0.139 g, 0.418 mmol), tetrakis(triphenylphosphine)palladium(0) (0.0241 g, 0.0209 mmol) and an aqueous saturated NaHCO3 solution (1 ml) in dioxane (4 ml), was heated at 150° C. for 10 min. under microwave irradiation. After cooling to r.t., the r.m. was filtered through diatomaceous earth, treated with EtOAc and the organic layer was washed with water and then with brine. The organic fraction was dried (Na2SO4), filtered and the solvent was evaporated in vacuo. The crude residue was purified by column chromatography (silica gel; 0-10% EtOAc/DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield D23 (0.027 g, 15.59%).

1. filtrationwas filtered through diatomaceous earth
2. additiontreated with EtOAc
3. washthe organic layer was washed with water
4. dry with materialThe organic fraction was dried (Na2SO4)
5. filtrationfiltered
6. customthe solvent was evaporated in vacuo
7. customThe crude residue was purified by column chromatography (silica gel; 0-10% EtOAc/DCM as eluent)
8. customThe desired fractions were collected
9. customevaporated in vacuo