反应详情

A solution of the product from Example 2 (100 mg) in THF (3 mL), under nitrogen, was treated with sodium hydride (60% in mineral oil) (10 mg). The suspension was stirred for 5 min were upon methoxyacetyl chloride (40 uL) was added. The reaction was allowed to warm to room temperature and was stirred 30 min. The reaction mixture was quenched with aqueous NaHCO3 (saturated) and extracted with ethyl acetate. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluted with 0-30% EtOAc in hexane afforded the title compound. HPLC/MS: 543.8 (M+1), 545.8 (M+3); Rt=4.19 min.

1. additionwas added
2. stirringwas stirred 30 min
3. customThe reaction mixture was quenched with aqueous NaHCO3 (saturated)
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by flash chromatography on silica
9. washeluted with 0-30% EtOAc in hexane