反应详情

A mixture of 6b (80 mg, 0.17 mmol), NaH (75 mg, 1.87 mmol) and DMF (1 mL) was stirred at room temperature for 30 minutes. Methyl iodide (0.025 mL, 0.4 mmol) was added and the mixture was heated at 90° C. in a sealed vial for 18 h. After cooling to room temperature, DCM (4 mL) and brine (4 mL) were added. The layers were separated and the aqueous layer was extracted with DCM (3×3 mL). The combined extracts were dried, filtered, evaporated and purified by preparative HPLC to give 16-1, LCMS 488.4 (MH+).

1. temperaturethe mixture was heated at 90° C. in a sealed vial for 18 h
2. temperatureAfter cooling to room temperature
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with DCM (3×3 mL)
5. customThe combined extracts were dried
6. filtrationfiltered
7. customevaporated
8. custompurified by preparative HPLC
9. customto give 16-1, LCMS 488.4 (MH+)