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 solution of tert-butyl {5-[2-(3-aminophenyl)ethyl]pyridin-3-yl}carbamate (0.50 g, 1.6 mmol) and 2,4,5-trichloropyrimidine (0.30 g, 1.6 mmol) in N,N-dimethylformamide (4 mL) was added potassium carbonate (0.43 g, 3.11 mmol). The resultant mixture was stirred overnight at room temperature. The reaction was quenched with water. EtOAc was added and the layers were separated. The aqueous layer was extracted with EtOAc once. The combined organic layers were washed with water and brine then dried (Na2SO4), filtered, and concentrated. The crude mixture was purified by silica gel column chromatography to give the desired product as a white powder (0.60 g, 82%). LCMS for C22H24Cl2N5O2 (M+H)+: m/z=460.1, 462.1.
WORKUP
后处理
- customThe reaction was quenched with water
- additionEtOAc was added
- customthe layers were separated
- extractionThe aqueous layer was extracted with EtOAc once
- washThe combined organic layers were washed with water and brine
- dry with materialthen dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude mixture was purified by silica gel column chromatography