反应详情

温度

90 °C

Zinc cyanide (1.1 g) and Pd(PPh3)4 (281 mg) were added to a DMF (45 mL) solution of methyl 5-{[(trifluoromethyl)sulfonyl]oxy}biphenyl-3-carboxylate (1.68 g), and stirred at 90° C. for 1 hour and 30 minutes. The reaction liquid was filtered through Celite, the solvent was partly evaporated away, and the residue was diluted with ethyl acetate, aqueous ammonia was added to it, and the solution was extracted with ethyl acetate. The organic layer was washed with water and saturated saline water, dried with anhydrous sodium sulfate, filtered, and the solvent was evaporated away. The residue was purified through silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound as a white powder.

1. customThe reaction liquid
2. filtrationwas filtered through Celite
3. customthe solvent was partly evaporated away
4. additionthe residue was diluted with ethyl acetate, aqueous ammonia
5. additionwas added to it
6. extractionthe solution was extracted with ethyl acetate
7. washThe organic layer was washed with water and saturated saline water
8. dry with materialdried with anhydrous sodium sulfate
9. filtrationfiltered
10. customthe solvent was evaporated away
11. customThe residue was purified through silica gel column chromatography (hexane/ethyl acetate)