反应详情

Sodium hydride (95%, 116 mg, 4.6 mmol) is suspended in 10 mL of anhydrous THF, and then a mixture of 1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione (300 mg, 1.65 mmol) and 1-(p-toluenesulfonyl)-ethyl isocyanide (413 mg, 1.98 mmol) in 5 mL of anhydrous THF is added dropwise over 1 h at 0° C. The mixture is stirred at room temperature for 3 h at room temperature after the completion of the addition, and then carefully quenched with water. The mixture is diluted with saturated NaHCO3, and then extracted with CH2Cl2 five times. The combined organic phase is washed with brine, and then dried with anhydrous Na2SO4. After filtration, the filtrate is evaporated to dryness under reduced pressure, and the residue is purified by basic alumina column chromatography to give 247 mg of product (yield: 64%). MS (ESI) m/z 236.1 [M+H]+.

1. additionis added dropwise over 1 h at 0° C
2. additionafter the completion of the addition
3. customcarefully quenched with water
4. additionThe mixture is diluted with saturated NaHCO3
5. extractionextracted with CH2Cl2 five times
6. washThe combined organic phase is washed with brine
7. dry with materialdried with anhydrous Na2SO4
8. filtrationAfter filtration
9. customthe filtrate is evaporated to dryness under reduced pressure
10. customthe residue is purified by basic alumina column chromatography