反应详情

温度

200 °C

To a stirred solution of ethyl 2-(6-(cyclopropylmethoxy)-5-iodo-4′-(trifluoromethyl)biphenyl-3-yl)-4-methylpentanoate (0.25 g, 0.447 mmol) in NMP (10 mL) was added CuCN (50 mg, 0.536 mmol) at RT under inert atmosphere. The reaction mixture was stirred at 200° C. temperature over a period of 2 h. After completion of starting material (by TLC), the reaction mixture was cooled to RT and extracted with EtOAc (3×20 mL). Combined organic layers were washed with water (3×15 mL), brine and dried over Na2SO4. After filtration and evaporation, the crude material was purified by column chromatography to afford ethyl 2-(5-cyano-6-(cyclopropylmethoxy)-4′-(trifluoromethyl)biphenyl-3-yl)-4-methylpentanoate (0.125 g) a solid.

1. temperatureAfter completion of starting material (by TLC), the reaction mixture was cooled to RT
2. extractionextracted with EtOAc (3×20 mL)
3. washCombined organic layers were washed with water (3×15 mL), brine
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration and evaporation
6. customthe crude material was purified by column chromatography