Reaktion #51890

Reaktionsgleichung

3-trifluoromethyl 4-fluoro-benzonitrile

diethanolamine

→

3-trifluoromethyl-4-[bis(2-hydroxyethyl)amino]benzonitrile

Lösungsmittel

N,N-dimethylacetamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was evaporated
2. 2
   Sonstigethe residue partitioned between CH2Cl2 (400 ml) and H2O (400 ml)
3. 3
   Trocknenthe organic layer dried (MgSO4)
4. 4
   Sonstigeevaporated to dryness
5. 5
   SonstigeThe residue was chromatographed

Vorschrift

A solution of 3-trifluoromethyl 4-fluoro-benzonitrile (9.45 g, 50 mmol) and diethanolamine (15.8 g, 0.15 mol) in N,N-dimethylacetamide (200 ml) was stirred for 7 days at 50° C. The solvent was evaporated, the residue partitioned between CH2Cl2 (400 ml) and H2O (400 ml), the organic layer dried (MgSO4) and evaporated to dryness. The residue was chromatographed using CH2Cl2-EtOH as eluent.

Quelle