反应详情

温度

60 °C

To a solution of 8-hydroxyquinaldic acid methyl ester (406 mg, 2 mmol, 1 eq.) and t-butyl-6-bromohexanoate (754 mg, 3 mmol, 1.5 eq.) in DMF (5 mL) was added potassium carbonate (828 mg, 6 mmol, 3 eq.). The mixture was stirred vigorously for 3 h at 60° C., and then concentrated in vacuo. The residue was diluted with ethyl acetate, washed with NaH2PO4 buffer (pH 5, 1M) and brine, dried over Na2SO4 and concentrated in vacuo. Crude product was purified by flash chromatography on silica using ethyl acetate:hexanes gradient to provide 617 mg of 1. Yield 86%. MS m/z 374 (M+H)+

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with ethyl acetate
3. washwashed with NaH2PO4 buffer (pH 5, 1M) and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customCrude product was purified by flash chromatography on silica