反应详情

49 g 1-Bromo-3-fluoro-4-trifluoromethoxybenzene was stirred into 100 mL dimethylacetamide together with 20 g copper(I)cyanide at 140° C. overnight. Additional 10 g copper cyanide was added and heating was continued at 150° C. for 4 h. Further 12 g copper cyanide was added and stirring continued at 150° C. overnight. After cooling, the mixture was filtered through Celite/Cellulose and washed with ethyl acetate. The filtrate was added to ice water and filtered again through Celite/Cellulose. The filtrate was extracted with ethyl acetate (×3), dried over magnesium sulfate and concentrated to provide a brown oil which was distilled at 7 mbar and 60° C. to yield two product fractions with 23.5 g and 12 g (content 80%) yield.

1. temperatureheating
2. waitcontinued at 150° C. overnight
3. temperatureAfter cooling
4. filtrationthe mixture was filtered through Celite/Cellulose
5. washwashed with ethyl acetate
6. additionThe filtrate was added to ice water
7. filtrationfiltered again through Celite/Cellulose
8. extractionThe filtrate was extracted with ethyl acetate (×3)
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated
11. customto provide a brown oil which
12. distillationwas distilled at 7 mbar and 60° C.
13. customto yield two product fractions with 23.5 g and 12 g (content 80%)
14. customyield