反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The N-(3-amino-2,4-difluorophenyl)-1-methyl-1H-imidazole-4-sulfonamide (45 mg, 0.16 mmol) prepared at Step 5 and the 6-(2-fluoropyridin-3-yl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purine (43 mg, 0.14 mmol) prepared at Step 7 were added and dissolved, and lithium (bistrimethylsilyl) amide (1.0M solution in THF) was applied slowly at 0° C. After stirring the reactant at room temperature for 1 hour, completing the reaction, pouring water, and extracting with ethylacetate, the organic layer was dried with sulfuric anhydride magnesium and vacuum concentrated, and then refined by means of column chromatography, so that 65 mg of the target compound, N-(2,4-difluoro-3-(3-(9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-yl)pyridin-2-ylamino)phenyl)-1-methyl-1H-imidazole-4-sulfonamide (percentage yield: 82%), was obtained.
WORKUP
后处理
- additionwere added
- dissolutiondissolved
- customwas applied slowly at 0° C
- customthe reaction
- extractionextracting with ethylacetate
- dry with materialthe organic layer was dried with sulfuric anhydride magnesium and vacuum
- concentrationconcentrated