反应详情

The bromide of Example 36 (1.50 g, 4.88 mmol) was taken up in dry DMF (40 ml) and treated with NaH (160 mg, 80% disp. in oil) at 0° C. The mixture was stirred at r.t. under nitrogen for 10 min, then KI (80 mg) added and the mixture heated at 70° C. for 4 h. The mixture was evaporated and partitioned between EtOAc and 1M HCl. The organic portion was washed with 5% KHCO3 and brine, filtered (Whatman® 1 PS, phase separator) and evaporated. The residue was chromatographed (eluant 2% MeOH in EtOAc) to provide a colourless oil (640 mg, 56%).

1. additionKI (80 mg) added
2. temperaturethe mixture heated at 70° C. for 4 h
3. customThe mixture was evaporated
4. custompartitioned between EtOAc and 1M HCl
5. washThe organic portion was washed with 5% KHCO3 and brine
6. filtrationfiltered (Whatman® 1 PS, phase separator)
7. customevaporated
8. customThe residue was chromatographed (eluant 2% MeOH in EtOAc)