反应详情

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.

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