4-Nitrophenyl methyl sulfide → HCID 59683178, Verbindung

HRID 548957

Reaktionsgleichung

Reaktionsgleichung von HRID 548957
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N-:11]Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.O.O.O.[Na+].[CH3:17][S:18][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1>C(#N)C.C(OCC)(=O)C>[CH3:17][S:18]([C:19]1[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=1)=[N:11][S:8]([C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][CH:4]=1)(=[O:10])=[O:9]

Komponenten

5

Edukt 2

HCID 961094-Nitrophenyl methyl sulfideHCID 517414chloramine-T trihydrate

Produkt 1

HCID 59683178HCID 59683178, VerbindungAusbeute 22 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

10.0 g (35.3 mmol) of chloramine-T trihydrate (Aldrich) are added to 5.0 g (29.6 mmol) of 1-methylsulphanyl-4-nitrobenzene in 120 ml of acetonitrile at room temperature. The mixture is stirred at room temperature for 4 hours and then diluted with ethyl acetate. The mixture is filtered with suction and the filter cake is washed with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated. The resulting residue is recrystallized from methanol. 2.2 g (6.5 mmol; yield: 22%) of the product are obtained.

Aufarbeitung

  1. filtrationThe mixture is filtered with suction
  2. washthe filter cake is washed with ethyl acetate
  3. dry with materialThe combined organic phases are dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting residue is recrystallized from methanol
  7. custom2.2 g (6.5 mmol; yield: 22%) of the product are obtained

Quellen und Nachweise

ORD-Eintrag
ord-46e8fd89e72b42cfa50550d8d73a9ec4
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07943629B2

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