反应详情

温度

100 °C

333.9 mg (2.4 mmol) 4-methyl-1H-pyrrole-3-carboxylic acid methyl ester, 891.5 mg (4.2 mmol) tri-potassium phosphate, 4 mg (0.02 mmol) CuI, 22 mg (0.2 mmol) 1,2-diaminocyclohexane and 317.9 mg (2 mmol) of 2-bromopyrimidine was suspended in 3 mL of dioxane. After addition of 90 μl of dodecane the mixture was heated in a sealed tube under argon for 12 h at 100° C. The mixture was cooled to room temperature and then diluted with water, followed by extraction with ethyl acetate. The organic layer was washed with water (twice), dried over anhydrous sodium sulfate. After filtration the solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column flash chromatography (eluent: heptane/dichloromethane/methanol=25/2/1) to obtain 300 mg of 4-Methyl-1-pyrimidin-2-yl-1H-pyrrole-3-carboxylic acid methyl ester as a white solid.

1. temperatureThe mixture was cooled to room temperature
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with water (twice),
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration the solvent
6. distillationwas distilled off under reduced pressure
7. customthe resulting residue was purified by a silica gel column flash chromatography (eluent: heptane/dichloromethane/methanol=25/2/1)