Isoamyl Nitrite → Ethyl [(4-chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}phenyl)thio]acetate

HRID 910836Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 910836
[SH:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].C(ON=O)CC(C)C.[Cl:16][C:17]1[CH:23]=[CH:22][C:20](N)=[C:19]([S:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH2:34][CH3:35])(=[O:33])=[O:32])=[CH:27][C:26]=2[Cl:36])[CH:18]=1>C(#N)C.O>[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([S:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:19]([S:24][C:25]2[CH:30]=[CH:29][C:28]([S:31]([CH2:34][CH3:35])(=[O:32])=[O:33])=[CH:27][C:26]=2[Cl:36])[CH:18]=1

Komponenten

6

Edukt 3

HCID 8053Isoamyl NitriteHCID 12185Ethyl ThioglycolateHCID 673913764-Chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}aniline

Produkt 1

HCID 86620103Ethyl [(4-chloro-2-{[2-chloro-4-(ethylsulfonyl)phenyl]thio}phenyl)thio]acetate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Ethyl mercaptoacetate (0.11 ml) followed by isoamylnitrite (0.16 ml) were added to a solution of the product from step (iii) (0.35 g) in dry acetonitrile (20 ml) and heated at 60° C. for 10 h. The mixture was diluted with water, extracted with diethylether, the organics dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with isohexane/diethylether 1:1, yield 0.10 g.

Aufarbeitung

  1. extractionextracted with diethylether
  2. customthe organics dried
  3. customevaporated under reduced pressure
  4. customThe residue was purified by chromatography on silica eluting with isohexane/diethylether 1:1, yield 0.10 g

Quellen und Nachweise

ORD-Eintrag
ord-ec67782cf61649b6a1a16fef9e985863
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08022248B2

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