تفاعل #158715

ord-00c388aa80c94cab8459db704ccb35b3

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822685B2uspto-grants-2014_09