Potassium nitrosodisulfonate → HCID 22506843, Verbindung

HRID 985571Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 985571
N(S([O-])(=O)=O)(S([O-])(=O)=[O:4])[O].[K+].[K+].[CH3:13][C:14]1([CH3:25])[CH2:22][C:21]2[C:16](=[C:17]([CH3:24])[CH:18]=[CH:19][C:20]=2[CH3:23])[NH:15]1>P([O-])([O-])([O-])=O.CO>[CH3:13][C:14]1([CH3:25])[CH2:22][C:21]2[C:16]([C:17]([CH3:24])=[CH:18][C:19](=[O:4])[C:20]=2[CH3:23])=[N:15]1

Komponenten

5

Edukt 2

HCID 3032624Potassium nitrosodisulfonateHCID 22506883HCID 22506883, Verbindung

Produkt 1

HCID 22506843HCID 22506843, VerbindungAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 1061PhosphateLösungsmittel

Versuchsvorschrift

To a solution of 65% potassium nitrosodisulfonate (10.4 g, 25.2 mmol) in pH 6.86 phosphate buffer (320 ml) was added a solution of 2,3-dihydro-2,2,4,7-tetramethyl-1H-indole (2.21 g, 12.6 mmol) in methanol (50 ml) and stirred at room temperature for 1.5 hours. The reaction mixture was extracted three times with toluene. The organic layers were combined, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was subjected to a column chromatography on a silica gel (hexane:ethyl acetate=5:1) and recrystallized from ethyl acetate-hexane to obtain 1.71 g of the title compound.

Aufarbeitung

  1. extractionThe reaction mixture was extracted three times with toluene
  2. washwashed with water and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customrecrystallized from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-966f2ea89d5f40ecbcad78287c321149
Quelldatensatz
uspto-grants-2005_03
Patentnummer
US06872718B1

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