Reaktion #59341
ord-2e78d71160104c28a4a102b782dcc95d
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe resulting mixture was heated
- 2Temperaturto reflux for 2 h and 40 minutes
- 3Sonstigefollowed by evaporation of the solvent under reduced pressure and treatment of the resulting yellow solid with 2M aqueous acetic acid (10 mL)
- 4Sonstigegiving a white solid
- 5FiltrationThe solid was collected by filtration
- 6Waschenwashed with 2M aqueous acetic acid (10 mL)
- 7Sonstigefollowed by evaporation
- 8Sonstigedrying under reduced pressure
Vorschrift
To 1-cyclopropylmethyl-2-thiourea (0.60 g, 4.6 mmol) in ethanol (10 mL) was added sodium methoxide (0.26 g, 4.8 mmol) and, after 5 minutes, ethyl cyanoacetate (0.50 mL, 4.6 mmol). The resulting mixture was heated to reflux for 2 h and 40 minutes followed by evaporation of the solvent under reduced pressure and treatment of the resulting yellow solid with 2M aqueous acetic acid (10 mL) giving a white solid. The solid was collected by filtration and washed with 2M aqueous acetic acid (10 mL), stirred with ethanol (10 mL) followed by evaporation and drying under reduced pressure, giving the title compound (0.51 g, 56%).