反应详情

温度

75 °C

To a stirred suspension of 30-35% KH (7.90 g) in 40 mL anhydrous diglyme at −20° C. was added a solution of diethoxyacetonitrile (Intermediate 1A, 6.20 g, 46.6 mmol) and methyl isocyanoacetate (4.96 g, 65.2 mmol) in 25 mL of anhydrous diglyme. The resulting mixture was heated to 70-80° C. and stirred overnight. The mixture was cooled to room temperature and quenched with saturated NH4Cl solution. DCM was added and the layers were separated. The mixture was further extracted with DCM. The combined organic extracts were dried over anhydrous MgSO4, filtered and concentrated under reduced pressure to give brown oil. Cold ether was added to the residue and the resulting white precipitate was filtered, washed with cold ether and dried to give the desired product Intermediate 1B (5.65 g, 53%) as a white solid.

1. temperatureThe mixture was cooled to room temperature
2. customquenched with saturated NH4Cl solution
3. additionDCM was added
4. customthe layers were separated
5. extractionThe mixture was further extracted with DCM
6. dry with materialThe combined organic extracts were dried over anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto give brown oil
10. filtrationthe resulting white precipitate was filtered
11. washwashed with cold ether
12. customdried