Potassium Hydroxide → HCID 87191335, Verbindung

HRID 2089002

Reaktionsgleichung

Reaktionsgleichung von HRID 2089002
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10](S(C3C=CC=CC=3)(=O)=O)[CH:9]=2)[CH:5]=[C:4]([Cl:26])[N:3]=1.[OH-].[K+]>C(O)C.O>[Cl:26][C:4]1[CH:5]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[NH:10][CH:9]=2)[CH:7]=[C:2]([Cl:1])[N:3]=1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 866498693-(2,6-dichloropyridin-4-yl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine

Produkt 1

HCID 87191335HCID 87191335, VerbindungAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 19096565Water ethanolLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

To a solution of Example 7a (5.72 g, 15 mmol) in 60 mL ethanol/water (5/1) was added powdered KOH (2 g, 35 mmol). The resulting solution was heated at 40° C. for 2 hours. Most of the solvent was removed in vacuo, and the residue was diluted with ethyl acetate. A solid was filtered from the material and discarded. The organics were washed with water, brine, dried over MgSO4, filtered, and concentrated. The crude material was triturated with dichloromethane and filtered, giving 3.5 g of the title compound as a white solid. MS (ESI+) m/z 263.6 (M+H)+.

Aufarbeitung

  1. customMost of the solvent was removed in vacuo
  2. additionthe residue was diluted with ethyl acetate
  3. filtrationA solid was filtered from the material
  4. washThe organics were washed with water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude material was triturated with dichloromethane
  9. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-dbe488fa85d8415a9d7ac19307942f55
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08435980B2

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