Potassium Carbonate → (S)-7-(2-hydroxyethyl)-9-neopentyl-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-one

HRID 2378613

Reaktionsgleichung

Reaktionsgleichung von HRID 2378613
C([O:4][CH2:5][CH2:6][C@H:7]1[C:20](=[O:21])[N:19]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:18][C:10]2[C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO>[OH:4][CH2:5][CH2:6][C@H:7]1[C:20](=[O:21])[N:19]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:18][C:10]2[C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8]1

Komponenten

4

Edukt 2

HCID 11430Potassium CarbonateHCID 59731999(S)-2-(9-neopentyl-8-oxo-3,6,7,8,9,10-hexahydroazepino[3,4-e]indazol-7-yl)ethyl acetate

Produkt 1

HCID 59731990(S)-7-(2-hydroxyethyl)-9-neopentyl-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-oneAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

(S)-2-(9-neopentyl-8-oxo-3,6,7,8,9,10-hexahydroazepino[3,4-e]indazol-7-yl)ethyl acetate (18 mg, 0.05 mmol) was dissolved in methanol (1 mL). Potassium carbonate (20 mg, 0.14 mmol) was added to the mixture. Reaction stirred at room temperature for 1 hour. Amberlite IRC-50 ion exchange resin was added to the mixture. Reaction stirred at room temperature for 15 minutes. Mixture was filtered. Filtrate was concentrated in vacuo. The title compound was obtained as yellow residue in 94% yield. MS m/e (M+H)+=316.

Aufarbeitung

  1. customReaction
  2. additionAmberlite IRC-50 ion exchange resin was added to the mixture
  3. customReaction
  4. stirringstirred at room temperature for 15 minutes
  5. filtrationMixture was filtered
  6. concentrationFiltrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9cb59c55a2964d1997489f75a6494b07
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07470679B2

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