Iodine → 1,9-Dimethylphenothiazin-5-ium iodide

HRID 72815

Reaktionsgleichung

Reaktionsgleichung von HRID 72815
[CH3:1][C:2]1[C:15]2[NH:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][C:12]=3[CH3:16])[S:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[I:17]I>C(Cl)(Cl)Cl>[I-:17].[CH3:16][C:12]1[C:13]2[C:8](=[S+:7][C:6]3[C:15]([N:14]=2)=[C:2]([CH3:1])[CH:3]=[CH:4][CH:5]=3)[CH:9]=[CH:10][CH:11]=1

Komponenten

4

Edukt 2

HCID 807IodineHCID 674644911,9-dimethyl-10H-phenothiazine

Produkt 1

HCID 890773051,9-Dimethylphenothiazin-5-ium iodide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

1,9-Dimethylphenothiazine (4.2026 g, 18.49 mmol) was dissolved in 130 mL of chloroform and crushed iodine (14.1 g, 55.55 mmol, 3 eq.) dissolved in 520 mL of chloroform was added over 2 hurs. Once newly formed precipitate was filtered off or the solvent removed under vacuum, the resulting iodide salt was stirred with ether or hexane (sometimes overnight) to remove excess iodine then refiltered. After pumping down under vacuum, a brown precipitate was obtained as product (12.6 g).

Aufarbeitung

  1. additionwas added over 2 hurs
  2. filtrationOnce newly formed precipitate was filtered off
  3. customthe solvent removed under vacuum
  4. customto remove excess iodine
  5. customa brown precipitate was obtained as product (12.6 g)

Quellen und Nachweise

ORD-Eintrag
ord-cedc4d50e13a4c5098b83e0fbcb6f8ee
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08828986B2

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