反应详情

温度

0 °C

To a solution of diisopropylamine (10.1 mL, 71.8 mmol) in anhydrous THF (50 mL) is added n-butyllithum (33.6 mL of an 1.6M in hexane) dropwise at 0° C. After 30 min at 0° C., 4-methyl-2-(methylthio)pyrimidine (5 mL, 35.9 mmol) is added. The resulting mixture is stirred at 0° C. for 30 min. After the addition of methyl isobutyrate (4.3 mL, 37.7 mmol) at 0° C., the reaction mixture is stirred overnight. The reaction mixture is quenched with acetic acid at 0° C., diluted with water, and extracted with ethyl ether. The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is purified by flash chromatography (SiO2, EtOAc/heptane 7:93 to 40:60) to give 4.3 g of 3-methyl-1-(2-methylsulfanyl-pyrimidin-4-yl)-butan-2-one.

1. stirringthe reaction mixture is stirred overnight
2. customThe reaction mixture is quenched with acetic acid at 0° C.
3. additiondiluted with water
4. extractionextracted with ethyl ether
5. dry with materialThe organic layer is dried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue is purified by flash chromatography (SiO2, EtOAc/heptane 7:93 to 40:60)