反应详情

温度

100 °C

To a solution of 0.149 g (0.35 mmol) of the product of Step G and 0.132 g (0.43 mmol) of t-butyl 2-iodobenzoate in 1 mL of anhydrous DMF was added 5 mg of bis(triphenylphosphine)palladium(II) chloride. The mixture was degassed, flushed with nitrogen, then magnetically stirred under a nitrogen atmosphere for 12 hours at 100° C. The reaction mixture was cooled to room temperature, then partitioned between EtOAc and water. The organic layer was extracted, separated, dried (MgSO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 50% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded 0.111 g (73%) of the title compound as an off-white amorphous solid.

1. customThe mixture was degassed
2. customflushed with nitrogen
3. temperatureThe reaction mixture was cooled to room temperature
4. custompartitioned between EtOAc and water
5. extractionThe organic layer was extracted
6. customseparated
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified on a silica gel flash chromatography column
11. washeluted with 50% EtOAc-hexane
12. customEvaporation of the purified fractions
13. customdrying in vacuo