反应详情

A 500 mL round bottom flask was charged with pent-4-ynyl-carbamic acid tert-butyl ester (1.35 g, 7.37 mmol), 4-amino-N-(3,4-dimethoxyphenyl)-3-iodobenzamide (1.35 g, 6.98 mmol), copper iodide (0.16 g, 0.814 mmol), palladium tetrakistriphenylphosphine (0.81 g, 0.701 mmol), and diethylamine (230 mL) and the resulting mixture stirred at room temperature for 24 h. The resulting mixture was then concentrated in vacuo and the residue purified via flash silica gel chromatography (Analogix IF-280, SF40-400 g column, gradient 90:10-10:90 Heptane:EtOAc) to yield {5-[2-amino-5-(3,4-dimethoxy-phenylcarbamoyl)-phenyl]-pent-4-ynyl}-carbamic acid tert-butyl ester. MS (ES+) 454 (M+1).

1. concentrationThe resulting mixture was then concentrated in vacuo
2. customthe residue purified via flash silica gel chromatography (Analogix IF-280