反应详情

First, 2-[2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]propionic acid (compound b-1) is dissolved in tetrahydrofuran, to which thionyl chloride is added under stirring, and the mixture is heated and stirred under reflux. After left for cooling and the subsequent concentration, the residue is dissolved in tetrahydrofuran (hereinafter referred to as solution A). Tetrahydrofuran is added to 1-pentyl alcohol, to which solution A id added and pyridine is then added. After stirring at room temperature, 2% aqueous hydrochloric acid is added to the reaction mixture, and the mixture is extracted with ethyl acetate. The organic layer is washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated. The residue is subjected to silica gel column chromatography (eluent: hexane/ethyl acetate=5/1) to give pentyl 2-[2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]propionate (compound b-19).

1. additionis added
2. temperaturethe mixture is heated
3. stirringstirred
4. temperatureunder reflux
5. waitAfter left
6. temperaturefor cooling
7. concentrationthe subsequent concentration
8. dissolutionthe residue is dissolved in tetrahydrofuran (
9. additionTetrahydrofuran is added to 1-pentyl alcohol, to which solution A id
10. additionadded
11. additionpyridine is then added
12. stirringAfter stirring at room temperature
13. addition2% aqueous hydrochloric acid is added to the reaction mixture
14. extractionthe mixture is extracted with ethyl acetate
15. washThe organic layer is washed with saturated aqueous sodium chloride solution
16. dry with materialdried over magnesium sulfate
17. concentrationconcentrated