反应详情

温度

60 °C

A mixture of methyl 3-bromo-6-bromomethyl-2-hydroxybenzoate (Intermediate 53, 0.6 g), 2-methoxythiophenol (0.518 g) and potassium carbonate (0.766 g) in THF (10 ml) was stirred and heated at 60° C. for 3 hours. After cooling, the mixture was partitioned between ethyl acetate and water and the separated organic layer was washed with potassium hydroxide solution, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-15% to give methyl 3-bromo-2-hydroxy-6-(2-methoxyphenylthiomethyl)-benzoate (0.46 g) as a white solid which was used without further characterisation.

1. temperatureAfter cooling
2. customthe mixture was partitioned between ethyl acetate and water
3. washthe separated organic layer was washed with potassium hydroxide solution
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customThe filtrate was evaporated to dryness
7. customthe residue was purified by chromatography on silica
8. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-15%