반응 #964435

반응 방정식

sodium hydroxide

ethyl 4,4,4-trifluoro-3-methyl-2-{4-[(5-oxo-2-phenyl-5,6-dihydro-4H-1,3,4-oxadiazin-4-yl)methyl]phenyl}butanoate

→

4,4,4-Trifluoro-3-methyl-2-{4-[(5-oxo-2-phenyl-5,6-dihydro-4H-1,3,4-oxadiazin-4-yl)methyl]phenyl}butanoic acid

용매

dioxane

반응 조건

후처리

1. 1
   기타the dioxane was removed under reduced pressure
2. 2
   workup.ADDITIONthe solution that remained was diluted with water
3. 3
   여과The precipitated solid was filtered off
4. 4
   세척washed with water
5. 5
   기타dried under reduced pressure at 45° C. overnight
6. 6
   workup.ADDITIONThis gave 1058 mg (2.52 mmol, 88% of theory) of the title compound as a mixture of isomers

실험 절차

11.4 ml (11.4 mmol) of 1 N aqueous sodium hydroxide solution were added to a solution of 1283 mg (2.86 mmol) of ethyl 4,4,4-trifluoro-3-methyl-2-{4-[(5-oxo-2-phenyl-5,6-dihydro-4H-1,3,4-oxadiazin-4-yl)methyl]phenyl}butanoate in 10 ml of dioxane, and the mixture was stirred at 80° C. overnight. After the reaction had gone to completion, the dioxane was removed under reduced pressure and the solution that remained was diluted with water and then adjusted to pH 2 using 1 M hydrochloric acid. The precipitated solid was filtered off, washed with water and dried under reduced pressure at 45° C. overnight. This gave 1058 mg (2.52 mmol, 88% of theory) of the title compound as a mixture of isomers.

출처