反应详情

{[1-(3,4-Difluoro-benzyl)-2-oxo-1,2-dihydro-pyridine-3-carbonyl]-amino}-thiophen-2-yl-acetic acid methyl ester (0.190 g, 0.000454 mol;) was dissolved in N,N-Dimethylformamide (6 mL, 0.07 mol;) and N-Bromosuccinimide (0.089 g, 0.00050 mol;) was added. The reaction was allowed to stir at room temperature o/n. LC-MS showed the formation of product at 1.89 498.45. The reaction was concentrated and dissolved in ethyl acetate. The reaction was then washed 1× with saturated bicarbonate and 1× with brine before drying with magnesium sulfate and concentrating. The crude was then dissolved in methylene chloride and injected onto the combiflash and eluted using a 0-100% hexanes ethyl acetate gradient. The pure fractions were combined and concentrated to give the product. ES (+) MS m/e=498.45

1. concentrationThe reaction was concentrated
2. dissolutiondissolved in ethyl acetate
3. washThe reaction was then washed 1× with saturated bicarbonate and 1× with brine
4. dry with materialbefore drying with magnesium sulfate
5. concentrationconcentrating
6. dissolutionThe crude was then dissolved in methylene chloride
7. washeluted
8. concentrationconcentrated
9. customto give the product