Reaktion #163826

ord-c8f766b2c54b40299c95e90185a4edfe

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was partitioned in 1N HCl solution (80 mL)
  2. 2
    ExtraktionThe aqueous layer was extracted with ethyl acetate (4×80 mL)
  3. 3
    SonstigeThe combined organic layers was dried
  4. 4
    Sonstigeevaporated
  5. 5
    Sonstigerecrystallized from MeOH/CH2Cl2/hexanes

Vorschrift

A mixture of 1,4-diaminobenzene (4 g, 37 mmol), ethyl isocyanate (1 mL, 12.6 mmol) and potassium carbonate (8.72 g, 63 mmol) in THF (20 mL) was stirred at room temperature overnight. The reaction mixture was partitioned in 1N HCl solution (80 mL) and ethyl acetate (80 mL). The aqueous layer was extracted with ethyl acetate (4×80 mL). The combined organic layers was dried, evaporated, recrystallized from MeOH/CH2Cl2/hexanes to give 4-(ethylaminocarbonylamino)aniline (1.4 g, 62%) as a beige solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835430B2uspto-grants-2014_09