反应详情

温度

75 °C

A mixture of diethoxyacetonitrile (38.72 mmol, 1 equiv.) and methyl isocyanoacetate (99.1 mmol, 1.4 equiv.) in dry bis(2-methoxyethyl)ether (20 ml) was added to a suspension of 30-35% KH (54.2 mmol, 1.4 equiv.) in dry bis(2-methoxyethyl)ether (30 ml). The resulting mixture was heated overnight at 70-80° C. The reaction mixture was then cooled to 25° C., and sat. NH4Cl solution (20 ml) was added. DCM (100 ml) was added, and the phases were separated. The aqueous phase was extracted with DCM (2×75 ml) and the combined organic phases were dried over Na2SO4 and filtered, and the solvent was removed in vacuo. Cold ether (10 ml) was added to the brown oil so obtained, and the resulting solid was filtered out and washed with ether. The desired product was thus obtained in the form of a yellow solid. Yield: 26%

1. temperatureThe reaction mixture was then cooled to 25° C.
2. customthe phases were separated
3. extractionThe aqueous phase was extracted with DCM (2×75 ml)
4. dry with materialthe combined organic phases were dried over Na2SO4
5. filtrationfiltered
6. customthe solvent was removed in vacuo
7. additionCold ether (10 ml) was added to the brown oil
8. customso obtained
9. filtrationthe resulting solid was filtered out
10. washwashed with ether