反应详情

温度

100 °C

A mixture of 280 mg (1.23 mmol) of 7-bromo-1-methyl-1,3-dihydro-2H-benzimidazol-2-one, 222 mg (1.48 mmol) of 2-ethylphenylboronic acid, 113 mg (0.0123 mmol) of tris(dibenzylideneacetone)dipalladium, 29 mg (0.0615 mmol) of X-Phos and 522 mg (2.46 mmol) of potassium phosphate in 9 mL of toluene was stirred at 100° C. for 4 hours. After cooling, the reaction mixture was diluted with water and ethyl acetate and passed through celite. The filtrate was extracted with ethyl acetate (X2). The combined organic layer was washed with brine (X1), dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 25-65% ethylacetate/n-hexane gradient mixture to give 200 mg (64%) of the title compound.

1. temperatureAfter cooling
2. extractionThe filtrate was extracted with ethyl acetate (X2)
3. washThe combined organic layer was washed with brine (X1)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel column chromatography
7. washeluting with a 25-65% ethylacetate/n-hexane gradient mixture