反应详情

温度

50 °C

Title compound 409 (0.403 g, 1.77 mmol) was dissolved in DMF (5.0 mL) and sodium hydride (60% in oil, 0.0.086 g, 2.13 mmol) was added. The reaction mixture was stirred at 50° C. for 30 minutes. Ethyl 7-bromoheptanoate (0.631 g, 2.66 mmol) was added and the reaction mixture was stirred at 50° C. for 16 hours. The mixture was cooled down to room temperature and quenched with water. The aqueous layer was extracted 3 times with at mixture of 75% ethyl acetate in hexanes. The combined organic extracts were washed with water and brine, dried over sodium sulfate, filtered and evaporated. The residue was purified by flash chromatography (30% ethyl acetate in hexanes) to afford title compound 410 (470 mg, 69%). MS (m/z): 384.4 (M+H).

1. stirringthe reaction mixture was stirred at 50° C. for 16 hours
2. temperatureThe mixture was cooled down to room temperature
3. customquenched with water
4. extractionThe aqueous layer was extracted 3 times
5. additionwith at mixture of 75% ethyl acetate in hexanes
6. washThe combined organic extracts were washed with water and brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified by flash chromatography (30% ethyl acetate in hexanes)