Reaktion #59341

ord-2e78d71160104c28a4a102b782dcc95d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe resulting mixture was heated
  2. 2
    Temperaturto reflux for 2 h and 40 minutes
  3. 3
    Sonstigefollowed by evaporation of the solvent under reduced pressure and treatment of the resulting yellow solid with 2M aqueous acetic acid (10 mL)
  4. 4
    Sonstigegiving a white solid
  5. 5
    FiltrationThe solid was collected by filtration
  6. 6
    Waschenwashed with 2M aqueous acetic acid (10 mL)
  7. 7
    Sonstigefollowed by evaporation
  8. 8
    Sonstigedrying 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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425560B2uspto-grants-2008_09