1-Chloro-2-(difluoromethyl)-4-nitrobenzene → 66351-92-6

HRID 891955Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 891955
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[CH:11]([F:13])[F:12]>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][C:3]=1[CH:11]([F:12])[F:13]

Komponenten

4

Edukt 1

HCID 222401911-Chloro-2-(difluoromethyl)-4-nitrobenzene

Produkt 1

HCID 2224027066351-92-6Ausbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
115 °C

Versuchsvorschrift

To a suspension of iron powder (16 g) in acetic acid (95 ml) was added 1-chloro-2-difluoromethyl-4-nitro-benzene (5.1 g, 15 mmol) and the reaction mixture was heated to 115° C. for 15 minutes. The mixture was filtered and the residue was washed with acetic acide and CH2Cl2. Evaporation of the solvent gave the crude product. It was further purified by chromatography over silica gel to give 4-chloro-3-difluoromethyl-phenylamine (76%), MS: m/e=177.1 (M+).

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. washthe residue was washed with acetic acide and CH2Cl2
  3. customEvaporation of the solvent
  4. customgave the crude product
  5. customIt was further purified by chromatography over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-9d5bf4bd1bef44b2a6acbe1fbb7d4dd3
Quelldatensatz
uspto-grants-2006_02
Patentnummer
US07005432B2

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