反应详情

To a degassed solution of the product mixture from Step 3 (320 mg, 0.64 mmol) in PhMe (5 mL) was added vinyltributyltin (0.225 mL, 0.77 mmol) and tetrakis(triphenylphosphine)palladium (74 mg, 0.06 mmol). The mixture was then heated to reflux for 18 h. The solvent was then removed in vacuo and the crude material was purified on silica (gradient elution, 5-50% EtOAc/hex) to provide the title compound as a 1:1 mixture with the expected regioisomer. LRMS ((M-Boc)+H)+=349.3.

1. temperatureThe mixture was then heated
2. temperatureto reflux for 18 h
3. customThe solvent was then removed in vacuo
4. customthe crude material was purified on silica (gradient elution, 5-50% EtOAc/hex)