反应详情

Under a nitrogen atmosphere (N2), HCOOH (2.44 g, 53 mmol) was added to Ac2O (6.48 g, 63.6 mmol) at 0° C. After it was allowed to warm to ambient temperature the reaction was heated at 50° C. for 15 hr. It was allowed to cool to ambient temperature. This mixed acid anhydride was then added dropwise to a solution of ethyl 2-amino-2-cyanoacetate (128 mg, 1 mmol) in dry THF (5 mL) at 0° C. After the cooling bath was removed, the reaction was maintained at ambient temperature for additional 1 hr. The reaction mixture was concentrated and purified by silica gel column chromatography (5:1 PE/EtOAc) to afford ethyl 2-cyano-2-formamidoacetate (110 mg, 70%) as a white solid.

1. temperaturewas heated at 50° C. for 15 hr
2. temperatureto cool to ambient temperature
3. customAfter the cooling bath was removed
4. temperaturethe reaction was maintained at ambient temperature for additional 1 hr
5. concentrationThe reaction mixture was concentrated
6. custompurified by silica gel column chromatography (5:1 PE/EtOAc)