反应详情

4-[1,2,3]Triazol-1-yl-benzoic acid (5.0 mmol) is dissolved in CH2Cl2 (20 ml). Oxalyl chloride (3.5 mmol) and DMF (1 drop) are added at room temperature and the reaction mixture is stirred at room temperature for 3 h, then evaporated. The residue is dissolved in CH2C2 (20 ml) and the mixture is added to 4-(2,2-dimethyl-propylamino)-5-ethynyl-pyrimidine-2-carbonitrile, copper (I) iodide (0.13 mmol) and triethylamine (13.0 mmol) at room temperature. The reaction mixture is stirred for overnight at room temperature. The organic layer is washed with brine, dried over magnesium sulfate and concentrated. The crude product is purified by silica gel column chromatography to give the product in 31% yield. Rf=0.02 (n-hexane:AcOEt=2:1)

1. customevaporated
2. dissolutionThe residue is dissolved in CH2C2 (20 ml)
3. stirringThe reaction mixture is stirred for overnight at room temperature
4. washThe organic layer is washed with brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe crude product is purified by silica gel column chromatography
8. customto give the product in 31% yield