반응 #51890

ord-02ab42cfd43b416bbf1faed23df2983f

반응 방정식

N#Cc1ccc(F)c(C(F)(F)F)c1
3-trifluoromethyl 4-fluoro-benzonitrile
OCCNCCO
diethanolamine
N#Cc1ccc(N(CCO)CCO)c(C(F)(F)F)c1
3-trifluoromethyl-4-[bis(2-hydroxyethyl)amino]benzonitrile

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated
  2. 2
    기타the residue partitioned between CH2Cl2 (400 ml) and H2O (400 ml)
  3. 3
    건조the organic layer dried (MgSO4)
  4. 4
    기타evaporated to dryness
  5. 5
    기타The residue was chromatographed

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06852755B1uspto-grants-2005_02