HRID2380955
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of N-(4-(2-(benzhydrylamino)-3-chloropyridin-4-yloxy)-3-fluorophenyl)-5-(4-fluorophenyl)-4-oxo-1,4-dihydropyridine-3-carboxamide (120 mg, 0.189 mmol), K2CO3 (104 mg, 0.756 mmol) and 1-tert-butyl 4-chloromethyl piperidine-1,4-dicarboxylate (157 mg, 0.567 mmol) in DMF (2 mL) was stirred at rt for 3 h. The reaction mixture was then diluted with DCM and the solid that formed was filtered off. The residue was washed with sat. aq. KH2PO4 solution. The organic layer was dried over MgSO4 and the desired product was purified by flash column chromatography (SiO2, eluting with a DCM/EtOAc gradient) to give the desired compound (145 mg) as a white solid. MS (ESI+) m/z 876 (M+H)+.
WORKUP
后处理
- customthe solid that formed
- filtrationwas filtered off
- washThe residue was washed with sat. aq. KH2PO4 solution
- dry with materialThe organic layer was dried over MgSO4
- customthe desired product was purified by flash column chromatography (SiO2
- washeluting with a DCM/EtOAc gradient)