反应详情

(Benzotriazol-1-yloxy)tripyrrolidino-phosphonium hexafluorophosphate (2.24 g, 4.30 mmol) was added to stirring suspension of (4-{[4-{[6-bromo-2-(methylcarbamoyl)pyridin-3-yl]amino}-5-(trifluoromethyl)pyrimidin-2-yl]amino}-3-methoxybenzyl)methylphosphinic acid (Compound 61B, 845 mg, 1.43 mmol), 3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl]propan-1-ol (Compound 3E, 362 mg, 1.43 mmol), and 1-methylimidazole (1.37 ml, 17.2 mmol) in 1,2-dichloroethane (31.2 ml) at 60° C. for 16 hrs. The reaction was quenched with water and extracted with EtOAc (3×), dried over sodium sulfate, filtered, and concentrated in vacuo and purified using a Teledyne ISCO Combiflash® Rf system [0→10% MeOH in 1:1 EtOAc/DCM] to afford 194 mg of the title compound as a racemic mixture (16%). MS (ESI): m/z=824.65 [M+H]+. UPLC: tR=1.17 min (UPLC-TOF: polar—2 min).

1. customThe reaction was quenched with water
2. extractionextracted with EtOAc (3×)
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. custompurified