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Sodium Hydroxide → HCID 19779367, Verbindung

HRID 1461731
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1461731
[Cl:1][C:2]1[C:3]([F:15])=[C:4]([N+:12]([O-])=O)[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[OH-].[Na+]>Cl>[NH2:12][C:4]1[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=[C:2]([Cl:1])[C:3]=1[F:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 27365653-Chloro-4-fluoro-5-nitrobenzotrifluoride

Produkt 1

HCID 19779367HCID 19779367, VerbindungAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

5-Chloro-4-fluoro-3-nitrotrifluoromethylbenzene (50 g) was added to a cooled (5° C.) solution of stannous chloride (140 g) in concentrated agueous hydrochloric acid (187 ml). After stirring for several hours at the ambient temperature (ca 22° C.), the reaction mixture was stood overnight. After basification by the addition of sodium hydroxide, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried, and the solvent removed by evaporation under reduced pressure. The residual yellow oil was kugelrohr distilled under reduced pressure to give 3-amino-5-chloro-4-fluorotrifluoromethylbenzene (32 g):bp. 105° C./11 mm Hg; 'H NMR δ (CDCl3) 7.03 (1H, dq), 6.90 (1H, dq).

Aufarbeitung

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. customthe solvent removed by evaporation under reduced pressure
  5. distillationThe residual yellow oil was kugelrohr distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-775e46c1ff9f4791ae7747f812f3f436
Quelldatensatz
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05077297

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