反应详情

温度

0 °C

A solution of the product from Example 2 (50 mg), potassium carbonate (14 mg) and benzyl bromide (12 μL) in THF (2 mL) was stirred overnight. No progress of the reaction was observed. The reaction mixture was cooled to 0° C., followed by addition of sodium hydride (60% in mineral oil) (4 mg). The reaction was stirred for 10 min and benzyl bromide (12 μL) was added. The suspension was allowed to come to room temperature and stirred overnight. The reaction was quenched with water and extracted twice with ethyl acetate. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated in vacuo. Purification on a preparative silica TLC plate eluted with 45% ethyl acetate in hexane afforded the title compound. HPLC/MS: 561.9 (M+1), 563.9 (M+3); Rt=5.09 min.

1. customto come to room temperature
2. stirringstirred overnight
3. customThe reaction was quenched with water
4. extractionextracted twice with ethyl acetate
5. washThe organic layer was washed with brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customPurification on a preparative silica TLC plate
10. washeluted with 45% ethyl acetate in hexane