反应详情

Sodium hydride (95%, 1.74 g, 69 mmol) is suspended in 20 mL of anhydrous THF, and then a mixture of 1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione (approx. 23 mmol) and p-toluenesulfonylmethyl isocyanide (97%, 7.0 g, 35 mmol) in 20 mL of anhydrous THF is added dropwise over 80 minutes at 0° C. The mixture is stirred at room temperature for an hour after the completion of the addition, and then carefully quenched with water. The mixture is diluted with 50 mL of 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 to give product as light brown solids, which is used for the next reaction without further purification. MS (ESI) m/z 222.2 [M+H]+.

1. additionis added dropwise over 80 minutes at 0° C
2. additionafter the completion of the addition
3. customcarefully quenched with water
4. additionThe mixture is diluted with 50 mL of 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. customto give product as light brown solids, which
11. customis used for the next reaction without further purification