反应详情

To a solution of the Grignard reagent derived from 2-(3-bromophenyl)-[1,3]dioxane (52.6 mL of 0.25M in THF, 13.1 mmol) at 0° C. was added copper (I) iodide (25 g, 13.1 mmol). After 45 minutes, 1,1,1-trifluoro-4-methylpent-3-en-2-one (2 g, 13.1 mmol) was added and the reaction mixture slowly warmed to room temperature and stirred overnight. The mixture was quenched with saturated aqueous ammonium chloride and extracted with ethyl acetate. The combined organic layers were washed with saturated aqueous sodium chloride solution, dried with sodium sulfate, and concentrated in vacuo. The residue was triturated with hexanes and filtered. The filtrate was concentrated in vacuo to give 4-(3-[1,3]dioxan-2-ylphenyl)-1,1,1-trifluoro-4-methylpentan-2-one.

1. customThe mixture was quenched with saturated aqueous ammonium chloride
2. extractionextracted with ethyl acetate
3. washThe combined organic layers were washed with saturated aqueous sodium chloride solution
4. dry with materialdried with sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was triturated with hexanes
7. filtrationfiltered
8. concentrationThe filtrate was concentrated in vacuo