反应详情

To a solution of 1-(azetidin-1-yl)-2-(2,6-difluoro-4-hydroxyphenyl)ethanone (50.0 mg, 0.128 mmol) in 5 ml anhydrous dichloromethane at RT was added a solution of 2-{(1S,2R)-2-[1-(5-ethylpyrimidin-2-yl)piperidin-4-yl]cyclopropyl}ethanol (38.0 mg, 0.182 mmol), triphenylphosphine (polymer-bound, 143 mg, 0.412 mmol), and di-tert-butyl azodicarboxylate (84.0 mg, 0.363 mmol). The reaction mixture was stirred at RT for 3 hours. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was filtered and purified by reverse-phase HPLC (SunFire Prep C18 OBD 5 um 19×100 mm column; 35-100% acetonitrile in 0.1% formic acid in water gradient), to give the title compound. LC/MS (m/z) 485.3 (M+H)+.

1. filtrationThe mixture was filtered through Celite
2. concentrationconcentrated under reduced pressure
3. filtrationThe residue was filtered
4. custompurified by reverse-phase HPLC (SunFire Prep C18 OBD 5 um 19×100 mm column; 35-100% acetonitrile in 0.1% formic acid in water gradient)