反应详情

To a cold (0° C.) solution of the amide 482 (328 mg, 1.0 mmol) in THF (20 mL) is added 0.5M 4-methoxyphenylmagnesium bromide in THF (8.0 mL, 4.0 mmol), and the mixture is allowed to come to rt and stirred at this temperature for 3 h. The reaction mixture is poured into a mixture of ammonium chloride/ice followed by the addition of EtOAc. The organic layer is separated, washed with brine, dried (MgSO4), and filtered. The filtrate is evaporated, and the residue purified by chromatography on silica gel; elution with heptane:EtOAc (85:15) gives 2.12 g of the product 483. 1H NMR (CDCl3) δ 7.95 (d, 2 H), 7.45-7.20 (m, 10 H), 6.88 (d, 2 H), 6.50-6.20 (m, 2 H), 5.25-5.00 (m, 2 H), 3.81 (s, 3 H)

1. customto come to rt
2. customThe organic layer is separated
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customThe filtrate is evaporated
7. customthe residue purified by chromatography on silica gel
8. washelution with heptane:EtOAc (85:15)