反应详情

First, 0.365 g of methyl 2-[2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]propionate was dissolved in 4 ml of 1,4-dioxane, to which a mixed solution of 1 ml of concentrated hydrochloric acid and 1 ml of water was added under stirring, and the mixture was heated and stirred under reflux for 5 hours and 45 minutes. The reaction mixture was then left for cooling, into which ice water was poured, and after addition of ethyl acetate and saturated aqueous sodium chloride solution, the mixture was subjected to phase separation. To the organic layer was added aqueous sodium hydrogencarbonate solution, and the mixture was subjected to phase separation. To the aqueous layer was added aqueous hydrochloric acid solution for acidification, to which ethyl acetate was added, and the mixture was subjected to phase separation. The organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated to give 0.183 g of 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.

1. additionwas added
2. temperaturethe mixture was heated
3. stirringstirred
4. temperatureunder reflux for 5 hours and 45 minutes
5. waitThe reaction mixture was then left
6. additionwas poured
7. customthe mixture was subjected to phase separation
8. additionTo the organic layer was added aqueous sodium hydrogencarbonate solution
9. customthe mixture was subjected to phase separation
10. additionTo the aqueous layer was added aqueous hydrochloric acid solution for acidification
11. additionto which ethyl acetate was added
12. customthe mixture was subjected to phase separation
13. washThe organic layer was washed with saturated aqueous sodium chloride solution
14. dry with materialdried over magnesium sulfate
15. concentrationconcentrated