反应详情

温度

40 °C

Subsequently, methyl 5-chloro-2-[3-(chloromethyl)benzoyl]-aminobenzoate (1.8 g) was dissolved in anhydrous methylene chloride. Triethylamine (1.5 ml) and 2-mercaptoethanesulfonic acid sodium salt (compound B′) (1.3 g) were added to the solution at room temperature, and the mixture was stirred at 40° C. for 4 days. After the completion of the reaction, distilled water was added thereto at room temperature, and the mixture was subjected to separatory extraction with chloroform. The organic layer was washed with a saturated aqueous sodium chloride solution, was dried over sodium sulfate, and was then concentrated. The residue was purified by column chromatography on silica gel to give 5-chloro-2-[3-(2-sulfo-ethylsulfanylmethyl)-benzoylamino]-benzoic acid methyl ester as a useful intermediate (1.08 g, yield 46.1%).

1. customAfter the completion of the reaction
2. distillationdistilled water
3. additionwas added
4. extractionat room temperature, and the mixture was subjected to separatory extraction with chloroform
5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
6. dry with materialwas dried over sodium sulfate
7. concentrationwas then concentrated
8. customThe residue was purified by column chromatography on silica gel