反应详情

A mixture of ethyl 2,4-dihydroxy-3-iodo-6-methylbenzoate (Intermediate 204, 0.144 g), dimethylsulphate (0.085 ml) and potassium carbonate (0.185 g) in acetone (10 ml) was heated at reflux for 2.5 hours. After cooling, the mixture was filtered and the filtrate was evaporated to dryness. The residue was partitioned between DCM and water and the organic layer was filtered through a phase separator. 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 0-20% to give ethyl 3-iodo-2,4-dimethoxy-6-methylbenzoate (0.158 g).

1. temperaturewas heated
2. temperatureat reflux for 2.5 hours
3. temperatureAfter cooling
4. filtrationthe mixture was filtered
5. customthe filtrate was evaporated to dryness
6. customThe residue was partitioned between DCM and water
7. filtrationthe organic layer was filtered through a phase separator
8. customThe filtrate was evaporated to dryness
9. customthe residue was purified by chromatography on silica
10. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-20%