반응 #51889

반응 방정식

3,5-difluoro-4-[bis(2-hydroxypropyl)amino]benzonitrile

NaOH

ethanol

→

3,5-difluoro-4-[bis(2-hydroxypropyl)amino]benzoic acid

반응 조건

후처리

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

실험 절차

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.

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