反应详情

温度

100 °C

A sealed tube was equipped with a magnetic stirrer and charged with 110e (740 mg, 3.6 mmol), 2,6-dibromo-4-fluorobenzyl acetate 101j (2.4 g, 7.2 mmol) and cesium carbonate (2.6 g, 7.9 mmol) in 1,4-dioxane (36 mL). After bubbling nitrogen through the solution for 30 min, Xantphos (250 mg, 0.43 mmol) and tris(dibenzylideneacetone) dipalladium(0) (260 mg, 0.29 mmol) were added, and the reaction mixture was heated to 100° C. for 16 h. After this time, H2O (50 mL) and ethyl acetate (50 mL) were added. The aqueous layer was separated and extracted with ethyl acetate (2×50 mL). The combined organic extracts were washed with brine (100 mL) and dried over sodium sulfate. The resulting residue was purified by column chromatography eluting with a gradient of 100% hexanes-100% Ethyl acetate to afford a 56% yield (910 mg) of 110f.

1. customA sealed tube was equipped with a magnetic stirrer
2. customAfter bubbling nitrogen through the solution for 30 min
3. customThe aqueous layer was separated
4. extractionextracted with ethyl acetate (2×50 mL)
5. washThe combined organic extracts were washed with brine (100 mL)
6. dry with materialdried over sodium sulfate
7. customThe resulting residue was purified by column chromatography
8. washeluting with a gradient of 100% hexanes-100% Ethyl acetate