Iodine chloride → 5-Chloro-2-iodo-4-(trifluoromethyl)aniline

HRID 2064128

Reaktionsgleichung

Reaktionsgleichung von HRID 2064128
[I:1]Cl.[Cl:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[NH2:7].O.O.O.C([O-])(=O)C.[Na+].C(=O)(O)[O-].[Na+].S([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C>[Cl:3][C:4]1[C:10]([C:11]([F:12])([F:13])[F:14])=[CH:9][C:8]([I:1])=[C:6]([CH:5]=1)[NH2:7]

Komponenten

6

Edukt 4

HCID 24640Iodine chlorideHCID 679623-Chloro-4-(trifluoromethyl)anilineHCID 18470521HCID 18470521, VerbindungHCID 23665404Sodium Acetate Trihydrate

Produkt 1

HCID 593205585-Chloro-2-iodo-4-(trifluoromethyl)aniline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Iodine monochloride (1.5 g) was added in one portion to a mixture of 3-chloro-4-trifluoromethylaniline (1.7 g), sodium acetate trihydrate (2.2 g), and acetic acid (10 ml) at room temperature. After 30 min aqueous sodium bicarbonate/sodium sulfite was added and the mixture extracted with diethyl ether. The organic phase was dried over Na2SO4, filtered and evaporated. The residue was purified by chromatography (ethyl acetate-hexane) to afford the title compound, 2.2 g.

Aufarbeitung

  1. extractionthe mixture extracted with diethyl ether
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was purified by chromatography (ethyl acetate-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-b60f57e2e4c145499e75c59bc916ea89
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288412B2

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