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

HRID 132424

Reaktionsgleichung

Reaktionsgleichung von HRID 132424
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-b566f640e1a0409aaf8a2f2fb9542367
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07384931B2

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