反应详情

温度

90 °C

A mixture of 3-[[2-chloro-4-pyridinyl]oxy]-1-naphthalenecarboxylic acid, methyl ester (0.188 g, 0.60 mmol), cyclopropanecarboxamide (0.077 g, 0.90 mmol), Cs2CO3 (0.274 g, 0.84 mmol), 1,1′-(9,9-dimethyl-9H-xanthene-4,5-diyl)bis[1,1-diphenylphosphine (0.035 g, 0.06 mmol; xantphos; Aldrich) and Pd2(dba)3 (0.018 g, 0.020 mmol) in dioxane (6 mL) is stirred at 90° C. for 16 h under an argon atmosphere. The cooled mixture is treated with saturated aqueous NH4Cl (50 mL) and extracted with ethyl acetate. The combined extracts are washed (brine), dried (Na2SO4) and the solvent is evaporated off under reduced pressure to give a crude product, which is purified by column chromatography (SiO2; ethylacetate/hexane 1:1) to afford the title compound as a viscous oil.

1. extractionextracted with ethyl acetate
2. washThe combined extracts are washed (brine)
3. dry with materialdried (Na2SO4)
4. customthe solvent is evaporated off under reduced pressure
5. customto give a crude product, which
6. customis purified by column chromatography (SiO2; ethylacetate/hexane 1:1)