反应详情
EQUATION
反应方程式
REACTANTS
反应物
Diisopropylethylamine
C8H19N
Sodium Bicarbonate
CHNaO3
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
1-(4-Fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid
C13H10FNO3
未命名化合物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To a solution of N-[6-(4-amino-2-chlorophenoxy)imidazo[1,2-a]pyridin-2-yl]cyclopropanecarboxamide (100 mg, 0.292 mmol) and 1-(4-fluorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid (94 mg, 0.38 mmol) in N,N-dimethylformamide (1 mL) were added N,N-diisopropylethylamine (100 μL, 0.583 mmol) and HATU (144 mg, 0.380 mmol), and the mixture was stirred at 60° C. for 4 hr. Ethyl acetate, tetrahydrofuran and saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and the mixture was extracted 3 times with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate alone) to give a white solid. The obtained solid was washed with ethyl acetate and collected by filtration to give the title compound (120.2 mg, 72%) as a white solid.
WORKUP
后处理
- extractionthe mixture was extracted 3 times with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography (ethyl acetate alone)
- customto give a white solid
- washThe obtained solid was washed with ethyl acetate
- filtrationcollected by filtration