反应详情

温度

100 °C

Into a sealed tube was charged with 334f (800 mg, 4 mmol) and 197c (3.8 g, 12 mmol) in dioxane (25 mL), and cesium carbonate (2.6 g, 8 mmol). After bubbling nitrogen through the resulting solution for 30 min, XantPhos (230 mg, 0.4 mmol) and tris(dibenzylideneacetone)-dipalladium(0) (362 mg, 0.4 mmol) were added, and the reaction mixture was heated at 100° C. for 4 h. After this time the reaction was cooled to room temperature, and partitioned between ethyl acetate (100 mL) and water (100 mL). The aqueous layer was separated and extracted with ethyl acetate (50 mL×3). The organic layers were combined, washed with brine (20 mL×3), and dried over sodium sulfate. The drying agent was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography eluting with 1:5 ethyl acetate/petroleum ether to give 334g as a brown solid (1.3 g, 72%). MS: [M+H]+ 447.

1. customAfter bubbling nitrogen through the resulting solution for 30 min
2. temperatureAfter this time the reaction was cooled to room temperature
3. custompartitioned between ethyl acetate (100 mL) and water (100 mL)
4. customThe aqueous layer was separated
5. extractionextracted with ethyl acetate (50 mL×3)
6. washwashed with brine (20 mL×3)
7. dry with materialdried over sodium sulfate
8. customThe drying agent was removed by filtration
9. concentrationthe filtrate was concentrated under reduced pressure
10. customThe residue was purified by column chromatography
11. washeluting with 1:5 ethyl acetate/petroleum ether