反应详情

温度

120 °C

A mixture of 2-(2-ethynylphenyl)propanamide K7 (0.120 g, 0.693 mmol), 4-chloro-N-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)pyrimidin-2-amine A68 (0.211 g, 0.693 mmol), CuI (0.013 g, 0.069 mmol), t-Bu3PHBF4 (0.020 g, 0.069 mmol) and PdCl2(PPh3)2 (0.024 g, 0.035 mmol) in DMF (3 mL) was bubbled with N2 for 5 minutes. Et3N (1 mL) was added and the reaction mixture was stirred in the microwave at 120° C. for 15 minutes. The volatiles were removed in vacuo and the black residue was adsorbed onto silica. Purification by column chromatography (Biotage Isolera, 40 g SiO2 cartridge, 0-100% EtOAc in petroleum benzine 40-60° C.) gave the title compound A69 as a yellow solid (0.198 g, 65%). LCMS-D: rt 3.43 min; m/z 442 [M+H]+.

1. customwas bubbled with N2 for 5 minutes
2. additionEt3N (1 mL) was added
3. customThe volatiles were removed in vacuo
4. customPurification by column chromatography (Biotage Isolera, 40 g SiO2 cartridge, 0-100% EtOAc in petroleum benzine 40-60° C.)