反应详情

温度

140 °C

To a mixture of 5-bromo-2-hydroxy-benzaldehyde (14 g, 70 mmol), KI (5 g) and K2CO3 (19 g, 140 mmol) in DMF (100 mL) was added toluene-4-sulfonic acid 3-methyl-oxetan-3-ylmethyl ester (18 g, 70 mmol). The mixture was heated at 140° C. for 2 h, and then cooled to room temperature, partitioned between water and ethyl acetate. The organic layer was washed with water for 3 times, dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give the title compound (10 g).

1. temperaturecooled to room temperature
2. custompartitioned between water and ethyl acetate
3. washThe organic layer was washed with water for 3 times
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by column chromatography