تفاعل #51889

ord-66ceef3ec995441e96eafebd7fc20035

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solution was partitioned between EtOAc (1.2 1) and HCl (500 ml, 0.4 M)
  2. 2
    غسيلthe aqueous layer washed with EtOAc (3×240 ml)
  3. 3
    تجفيفthe combined organic layers dried (MgSO4)
  4. 4
    أخرىevaporated to dryness
  5. 5
    أخرىThe residue was chromatographed

الإجراء التجريبي

A solution of the 3,5-difluoro-4-[bis(2-hydroxypropyl)amino]benzonitrile and NaOH (8 g, 0.2 mol) in aqueous ethanol (100 ml, 50%) was refluxed for 2.5 hours. The solution was partitioned between EtOAc (1.2 1) and HCl (500 ml, 0.4 M), the aqueous layer washed with EtOAc (3×240 ml), the combined organic layers dried (MgSO4) and evaporated to dryness. The residue was chromatographed using CH2Cl2-EtOH-ACOH as eluent.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06852755B1uspto-grants-2005_02