反应详情

To a stirred solution of 1.87 g (3.9 mmol) of the product of Step B in 24 mL of DMF at 0° C. was added 7.9 mL of a 1.0 M solution of lithium bis(trimethylsilyl)amide in THF. The reaction mixture was stirred an addition 5 min then it was quenched with 0.45 mL of acetic acid and then partitioned between ethyl acetate and saturated NaCl solution. The organic layer was separated, dried (MgSO4), filtered and evaporated. The residue was then purified via silica gel flash chromatography eluting with a gradient of 0 to 40% ethyl acetate/hexane to afford the title compound. HPLC/MS: 475.1 (M+1), 477.0 (M+3); Rt=3.99 min.

1. additionan addition 5 min
2. customit was quenched with 0.45 mL of acetic acid
3. custompartitioned between ethyl acetate and saturated NaCl solution
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customThe residue was then purified via silica gel flash chromatography
9. washeluting with a gradient of 0 to 40% ethyl acetate/hexane