反应详情

11.5 g (60 mmol) of a 28% sodium methoxide solution was dissolved in 100 ml of methanol, and 5.6 g (54 mmol) of formamidine acetate was added, followed by stirring at room temperature for 15 minutes. Then, 11.5 g (54 mmol) of 4-ethoxymethylene-2,6-dimethyl-3,5-heptanedione was added under cooling with ice. The reaction mixture was further reacted at 50° C. for one hour. The solvent was distilled off under reduced pressure, and 200 ml of water was added, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=4:1) to obtain 9.2 g (yield: 89%) of 5-isopropylcarbonyl-4-isopropylpyrimidine as slightly yellow liquid.

1. temperatureunder cooling with ice
2. customThe reaction mixture was further reacted at 50° C. for one hour
3. distillationThe solvent was distilled off under reduced pressure, and 200 ml of water
4. additionwas added
5. extractionfollowed by extraction with ethyl acetate
6. washThe obtained organic layer was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationEthyl acetate was distilled off under reduced pressure
9. customthe residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=4:1)