HCID 23031086, Verbindung → HCID 23031257, Verbindung

HRID 1766676Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1766676
FC(F)(F)S(O[C:7]1[C:15]([CH3:16])=[CH:14][C:13]([N+:17]([O-:19])=[O:18])=[C:12]2[C:8]=1[CH2:9][CH2:10][CH2:11]2)(=O)=O.O.[I-:23].[Li+]>CN(C)C=O>[I:23][C:7]1[C:15]([CH3:16])=[CH:14][C:13]([N+:17]([O-:19])=[O:18])=[C:12]2[C:8]=1[CH2:9][CH2:10][CH2:11]2

Komponenten

4

Edukt 2

HCID 23031086HCID 23031086, VerbindungHCID 23688290LITHIUM IODIDE

Produkt 1

HCID 23031257HCID 23031257, VerbindungAusbeute 77,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

To a solution of 5-methyl-7-nitroindan-4-yl trifluoromethanesulfonate (3.02 g) in N,N-dimethylformamide (10 mL) was added lithium iodide mono hydrate (6.10 g). The mixture was stirred under an argon atmosphere at 150° C. for 7 hours. Adding water, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with a 1 mol/L aqueous solution of sodium hydroxide, water and brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (2.19 g).

Aufarbeitung

  1. extractionAdding water, the reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with a 1 mol/L aqueous solution of sodium hydroxide, water and brine successively
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d7861d79d19e4ebb8d3744b70f930fe5
Quelldatensatz
uspto-grants-2007_06
Patentnummer
US07230031B2

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