反应详情

温度

100 °C

A mixture of 1-(2-chloro-4-pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene (22.7 g), phosphorus tribromide (52 ml) and 1,1,2,2-tetrachloroethane (100 ml) is stirred at 100° C. for 10 hours. After the reaction is complete, the mixture is concentrated under reduced pressure to remove the solvent, and thereto are added methylene chloride and an aqueous potassium carbonate solution. The methylene chloride layer is separated, and concentrated under reduced pressure to remove the solvent. The residue is crystallized from methanol to give 1-(2-bromo-4-pyridyl)-2,3-bis(methoxycarbonyl)-6,7-dimethoxynaphthalene (17.1 g).

1. concentrationthe mixture is concentrated under reduced pressure
2. customto remove the solvent
3. additionare added methylene chloride
4. customThe methylene chloride layer is separated
5. concentrationconcentrated under reduced pressure
6. customto remove the solvent
7. customThe residue is crystallized from methanol