반응 #75119

ord-0fc569756f4846f6bd4dc3333afcf253

반응 방정식

O=[N+]([O-])c1cc(C(F)(F)F)ccc1Cl
1-chloro-2-nitro-4-(trifluoromethyl)benzene
NCCCO
3-amino-1-propanol
O=[N+]([O-])c1cc(C(F)(F)F)ccc1NCCCO
3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol
수율 100.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도till reflux
  3. 3
    workup.STIRRINGStirring
  4. 4
    온도at reflux
  5. 5
    온도The reaction mixture is cooled
  6. 6
    기타evaporated
  7. 7
    workup.ADDITIONWater is added to the residue
  8. 8
    추출The product is extracted with methylbenzene
  9. 9
    기타The extract is dried
  10. 10
    여과filtered
  11. 11
    기타evaporated
  12. 12
    기타The solid residue is crystallized from petroleumether
  13. 13
    여과The product is filtered off
  14. 14
    기타dried

실험 절차

A mixture of 100 parts of 1-chloro-2-nitro-4-(trifluoromethyl)benzene, 90 parts of 3-amino-1-propanol and 200 parts of butanol is stirred and heated till reflux. Stirring at reflux is continued overnight. The reaction mixture is cooled and evaporated. Water is added to the residue and the whole is acidified with a hydrochloric acid solution. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The solid residue is crystallized from petroleumether. The product is filtered off and dried, yielding 141 parts (100%) of 3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04175129uspto-grants-1979_11