反应详情

A solution of Example 1B (1.09 g, 3.07 mmoles) in tetrahydrofuran (3.5 mL) was added drop wise to a solution of lithium bis(trimethylsilyl)amide in tetrahydrofuran (3.7 mL, 3.7 mmoles) at room temperature and stirred for two hours at that temperature. A solution of methyl iodide (0.54 g, 3.83 mmoles) in tetrahydrofuran (1 mL) was added drop wise to the reaction mixture at room temperature and stirred for another two hours. The reaction was quenched with 10% NH4Cl (25 mL) and extracted with ethyl acetate. The organic layer was washed with brine (25 mL), dried with MgSO4, filtered, and solvent evaporated in vacuo. The crude product was purified by flash column chromatography (hexanes:ethyl acetate 95:5 to 60:40) to provide the title compound.

1. stirringstirred for another two hours
2. customThe reaction was quenched with 10% NH4Cl (25 mL)
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with brine (25 mL)
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. customsolvent evaporated in vacuo
8. customThe crude product was purified by flash column chromatography (hexanes:ethyl acetate 95:5 to 60:40)