Reacción #158715

ord-00c388aa80c94cab8459db704ccb35b3

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08822685B2uspto-grants-2014_09