反应详情

温度

0 °C

To a 0° C. solution of methanol (50 mL) and 5-formyl-2-hydroxy-benzamide (Reich et al. J. Med. Chem., 2000;43(9):1670–1683) (2.0 g, 12.11 mmol) was added potassium hydroxide (1.35 g, 24.22 mmol) and then iodobenzene diacetate (3.90 g, 12.11 mmol). The reaction was stirred at 0° C. for 1 hour, then diluted with ethyl acetate (200 mL) and carefully acidified to pH 2 with 1N HCl. The organic layer was then washed with sodium chloride (2×50 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure. This was used in the next step without purification. MS: M+−1=162.0 Da.

1. washThe organic layer was then washed with sodium chloride (2×50 mL)
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThis was used in the next step without purification