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 25 mL microwave tube containing N-(2-chloro-3-nitropyridin-4-yl)-2,6-dichloro-4-cyanobenzamide (100 mg, 0.27 mmol), 2,6-dimethylpyrimidin-4-amine (43 mg, 0.35 mmol), Pd2(dba)3 (8 mg, 0.009 mmol), Cs2CO3 (180 mg, 0.54 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos, 4 mg, 0.005 mmol), dioxane (8 mL) and DME (3 mL) was degassed and then charged by N2 (3×). The mixture was then irradiated in a microwave reactor at 160° C. for 2 hours and then diluted with dioxane (20 mL). The reaction was filtered through Celite and concentrated under reduced pressure. The residue was purified by reverse-phase HPLC (Gemini, 200 mm×25 mm, gradient: CH3CN/0.05% NH3.H2O, 50-80, 10 min) to afford the desired product (4 mg, yield: 5%). LCMS (ESI) m/z: 458.3 [M+H+].
WORKUP
后处理
- customwas degassed
- additioncharged by N2 (3×)
- customThe mixture was then irradiated in a microwave reactor at 160° C. for 2 hours
- additiondiluted with dioxane (20 mL)
- filtrationThe reaction was filtered through Celite
- concentrationconcentrated under reduced pressure
- customThe residue was purified by reverse-phase HPLC (Gemini, 200 mm×25 mm, gradient: CH3CN/0.05% NH3.H2O, 50-80, 10 min)