反应详情
EQUATION
反应方程式
REACTANTS
反应物
N,N-Dimethylformamide
C3H7NO
Diisopropylethylamine
C8H19N
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
1-[(3,4-Difluorophenyl)methyl]-2-oxo-1,2-dihydropyridine-3-carboxylic acid
C13H9F2NO3
未命名化合物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
C-{5-[1-(2-Trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-thiophen-2-yl}-methylamine (23 mg, 0.000064 mol), 1-(3,4-difluoro-benzyl)-2-oxo-1,2-dihydro-pyridine-3-carboxylic acid (2.0E1 mg, 0.000075 mol) and HATU (44 mg, 0.00012 mol; Applied Biosystems) were dissolved in N,N-dimethylformamide (1.25 mL, 0.0161 mol; Acros). To this was added N,N-diisopropylethylamine (56 uL, 0.00032 mol; Aldrich) and the reaction was stirred for 1 hour at room temperature. The reaction was diluted with 5% citric acid in water, then extracted with ethyl acetate. Saturated sodium chloride was added to aid separation. The organic layer was washed with saturated sodium chloride, dried with sodium sulfate, filtered and evaporated to yield the crude title compound. MS m/z=608.34 (M+1).
WORKUP
后处理
- extractionextracted with ethyl acetate
- additionSaturated sodium chloride was added
- customseparation
- washThe organic layer was washed with saturated sodium chloride
- dry with materialdried with sodium sulfate
- filtrationfiltered
- customevaporated