反应详情

A mixture of 1.2 g (0.0023 mole) of t-butyl 2-[2-[2-chloro-4-fluoro-5-(4-difluoromethyl -4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]pyridin-5-yloxy]propionate (prepared by the method of Example 3, Step E using t-butyl 2-chloropropionate) in 7 mL of trifluoroacetic acid was stirred at room temperature for 30 minutes. The excess trifluoroacetic acid was removed by evaporation under reduced pressure leaving an oil. The oil was partitioned between diethyl ether and water. The organic phase was separated, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated under reduced pressure leaving a thick oil. Upon standing, the oil crystallized as a white solid. The solid was triturated with petroleum ether to give 0.66 g of 2-[2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]pyridin-5-yloxy]propionic acid, m.p. 49°-51° C.

1. customprepared by the method of Example 3, Step E
2. customThe excess trifluoroacetic acid was removed by evaporation under reduced pressure
3. customleaving an oil
4. customThe oil was partitioned between diethyl ether and water
5. customThe organic phase was separated
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customThe filtrate was evaporated under reduced pressure
9. customleaving a thick oil
10. customthe oil crystallized as a white solid
11. customThe solid was triturated with petroleum ether