反应详情

A solution of 1-(2-((2-((6-methoxypyridin-3-yl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethynyl)phenyl)cyclopropanecarboxamide A73 (0.229 g, 0.505 mmol) in EtOAc (20 mL) was stirred over 10% Pd/C (wetted with ca. 53% water, 0.150 g) under an atmosphere of hydrogen for 16 hours. The mixture was filtered through Celite and the solvent was removed in vacuo. Purification by column chromatography (Biotage Isolera, 40 g SiO2, 0-80% EtOAc in petroleum benzine 40-60° C.) gave an off-white solid contaminated with alkyne starting material. The solid was dissolved in EtOAc (20 mL) and MeOH (10 mL) and stirred over 10% Pd/C (wetted with ca. 53% water, 0.130 g) for 16 hours under an atmosphere of hydrogen. The mixture was filtered through Celite and the solvent was removed in vacuo to give the title compound 64 as a white solid (0.130 g, 56%). LCMS-D: rt 3.51 min; m/z 458 [M+H]+.

1. filtrationThe mixture was filtered through Celite
2. customthe solvent was removed in vacuo
3. customPurification by column chromatography (Biotage Isolera, 40 g SiO2, 0-80% EtOAc in petroleum benzine 40-60° C.)
4. customgave an off-white solid
5. filtrationThe mixture was filtered through Celite
6. customthe solvent was removed in vacuo