反应详情

2-Hydroxy-4-iodo-benzylalcohol from Step 3 (1.0 g, 4.0 mmol), Cs2CO3 (1.3 g, 4.0 mmol) and iodomethane (0.25 mL, 4.0 mmol) were dissolved in DMF and heated to 80° for 1 hour and then stirred at room temperature for 2 hours. The DMF was removed in vacuo and the residue was partitioned between H2O and EtOAc. The aqueous layer was extracted with EtOAc (2×). The organic layers were combined, washed with H2O and brine, dried (MgSO4), filtered and concentrated to yield an oil. This oil was purified by flash chromatography eluting product with 30% EtOAC/Hexane to give the title compound.

1. temperatureheated to 80° for 1 hour
2. customThe DMF was removed in vacuo
3. customthe residue was partitioned between H2O and EtOAc
4. extractionThe aqueous layer was extracted with EtOAc (2×)
5. washwashed with H2O and brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customto yield an oil
10. customThis oil was purified by flash chromatography
11. washeluting product with 30% EtOAC/Hexane