反应详情

(5-Chloro-2-iodo-phenyl)-(2,6-difluoro-phenyl)-methanone (2aa) (5.5 g, 14.5 mmol), prop-2-ynyl-carbamic acid tert-butyl ester (2.5 g, 16 mmol), PdCl2 (PPh3)2 (0.6 g, 0.9 mmol) and Cu(I)I (0.2 g, 0.9 mmol) were suspended in anhydrous CH2Cl2 (50 mL) and the mixture was sparged with nitrogen for 30 min. Diethylamine (8 mL) was added and the solution was stirred at room temperature for 16 h. The solution was concentrated in vacuo and the resulting residue purified by column chromatography (silica gel, 0 to 15% EtOAc/hexanes) to afford 3aa (3.6 g, 61%) as a white solid, MS m/z=406 (M+H).

1. customthe mixture was sparged with nitrogen for 30 min
2. additionDiethylamine (8 mL) was added
3. concentrationThe solution was concentrated in vacuo
4. customthe resulting residue purified by column chromatography (silica gel, 0 to 15% EtOAc/hexanes)
5. customto afford 3aa (3.6 g, 61%) as a white solid, MS m/z=406 (M+H)