Water → 4-Trifluoromethyl-1,2-phenylenediamine

HRID 53817

Reaktionsgleichung

Reaktionsgleichung von HRID 53817
[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:5]=1[NH2:6])([O-])=O.Cl[Sn]Cl.O.C([O-])(O)=O.[Na+]>C(O)C>[F:12][C:11]([F:13])([F:14])[C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([NH2:1])[CH:10]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 24479Stannous ChlorideHCID 67865Benzenamine, 2-nitro-4-(trifluoromethyl)-HCID 516892Sodium Bicarbonate

Produkt 1

HCID 5208224-Trifluoromethyl-1,2-phenylenediamineAusbeute 96,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-nitro-4-trifluoromethylaniline (5.000 g, 24.26 mmol, Aldrich, used as received) and SnCl2.2 H2O (20.00 g, 88.64 mmol, Aldrich, used as received) in absolute ethanol (50 mL) was refluxed for 45 min. It was then poured into ice (85 g) and basified with 10% aq. NaHCO3 (250 mL). The resulting suspension was extracted with ethyl acetate (400 mL). The ethyl acetate extract was dried over Na2SO4 and evaporated to give 4.14 g (87%) of pure 4-trifluoromethyl-1,2-phenylenediamine as a red powder.

Aufarbeitung

  1. extractionThe resulting suspension was extracted with ethyl acetate (400 mL)
  2. extractionThe ethyl acetate extract
  3. dry with materialwas dried over Na2SO4
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-87709eac85a547ac97c7cbd71cbdd542
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620979

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