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
To a mixture comprising tert-butyl 8-bromo-2,3-diphenyl-7,8-dihydropyrido[2,3-b]pyrazine-5(6H)-carboxylate (Intermediate H) (200 mg, 0.429 mmol) and silver nitrate (0.728 mg, 4.29 μmol) in diethyl ether (4 ml) under nitrogen at RT was added 1-Methylmagnesium bromide in THF (0.557 ml, 0.557 mmol). The reaction mixture was left to stir at RT for 3 h under an atmosphere of nitrogen. The mixture was poured into a saturated ammonium chloride solution (10 ml) and extracted with EtOAc (2×10 ml). The organic extracts were combined, dried over MgSO4, filtered and concentrated in vacuo. The resulting crude product was purified by chromatography on silica eluting with 0-30% EtOAc/iso-hexane to afford the title compound;
WORKUP
后处理
- waitThe reaction mixture was left
- extractionextracted with EtOAc (2×10 ml)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting crude product was purified by chromatography on silica eluting with 0-30% EtOAc/iso-hexane