4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene → 1-Propanol, 3-[[2-nitro-4-(trifluoromethyl)phenyl]amino]-

HRID 46841

Reaktionsgleichung

Reaktionsgleichung von HRID 46841
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[NH2:15][CH2:16][CH2:17][CH2:18][OH:19]>C(O)CCC>[N+:12]([C:3]1[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=1[NH:15][CH2:16][CH2:17][CH2:18][OH:19])([O-:14])=[O:13]

Komponenten

4

Edukt 2

HCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 90863-Amino-1-propanol

Produkt 1

HCID 28475091-Propanol, 3-[[2-nitro-4-(trifluoromethyl)phenyl]amino]-Ausbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperatureheated
  2. temperaturetill reflux
  3. stirringStirring
  4. temperatureat reflux
  5. temperatureThe reaction mixture is cooled
  6. customevaporated
  7. additionWater is added to the residue
  8. extractionThe product is extracted with methylbenzene
  9. customThe extract is dried
  10. filtrationfiltered
  11. customevaporated
  12. customThe solid residue is crystallized from petroleumether
  13. filtrationThe product is filtered off
  14. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0fc569756f4846f6bd4dc3333afcf253
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04175129

Verknüpfte Notizen

Wird geladen…