StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Dimethyl Sulfoxide → N-(6-(6-chloro-5-(methylsulfonamido)pyridin-3-yl)imidazo[1,2-b]pyridazin-2-yl)acetamide

HRID 1162450
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1162450
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([NH:11][C:12](=[O:14])[CH3:13])[N:10]=2)[N:7]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.CS(C)=O.C([O-])(=O)C.[K+].Br[C:43]1[CH:44]=[C:45]([NH:50][S:51]([CH3:54])(=[O:53])=[O:52])[C:46]([Cl:49])=[N:47][CH:48]=1.C(=O)([O-])[O-].[Na+].[Na+].C([O-])(=O)C.[Na+]>O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Cl:49][C:46]1[N:47]=[CH:48][C:43]([C:2]2[CH:3]=[CH:4][C:5]3[N:6]([CH:8]=[C:9]([NH:11][C:12](=[O:14])[CH3:13])[N:10]=3)[N:7]=2)=[CH:44][C:45]=1[NH:50][S:51]([CH3:54])(=[O:53])=[O:52]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 7

HCID 679Dimethyl SulfoxideHCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 517045Sodium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 59519510N-(6-chloroimidazo[1,2-b]pyridazin-2-yl)acetamide
HCID 59519513
N-(5-bromo-2-chloro-3-pyridinyl)methanesulfonamide

Produkt 1

HCID 44125613N-(6-(6-chloro-5-(methylsulfonamido)pyridin-3-yl)imidazo[1,2-b]pyridazin-2-yl)acetamideAusbeute 31,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418476HCID 178418476, VerbindungKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To a 25 mL round-bottomed flask was added N-(6-chloroimidazo[1,2-b]pyridazin-2-yl)acetamide (0.750 g, 3.56 mmol), bis(pinacolato)diboron (1.18 g, 4.63 mmol, Aldrich, St. Louis, Mo.), DMSO (30.0 mL, 423 mmol) and potassium acetate (1.40 g, 14.2 mmol). The mixture was carefully evacuated and backfilled with N2. To the mixture was added dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II)dichloromethane adduct (0.291 g, 0.356 mmol, Strem Chemical, Inc., Newburyport, Mass.). The mixture was carefully evacuated and backfilled with N2 and then was stirred at 90° C. for 2 h. The reaction was allowed to cool to rt and treated with N-(5-bromo-2-chloropyridin-3-yl)methanesulfonamide (1.00 g, 3.50 mmol), and aq sodium carbonate (5.25 mL, 10.5 mmol, 2 M). The mixture was carefully evacuated and backfilled with N2. To the mixture was added trans-dichlorobis(triphenylphosphine)palladium(II) (0.246 g, 0.350 mmol, Strem Chemical, Inc., Newburyport, Mass.). Again, the mixture was carefully evacuated and backfilled with N2 and was stirred at 90° C. for 1 h. The reaction mixture was cooled to rt and concentrated in vacuo. The residue was taken up in 10 mL DMSO and 20 mL MeOH. The solution was filtered. The filtercake was isolated and suspended in water (50 mL) and treated with pH 4.8 buffer (25 mL, Teknova, 3 M sodium acetate solution pH adjusted to 4.8). The solution was allowed to stand for 30 minutes and then filtered. The filtercake was washed with water and then dried under vacuum to afford the title compound as a tan solid (0.415 g, 31%). MS (ESI, positive ion) m/z: 381 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.12 (s, 3H), 3.17 (s, 3H), 7.85 (d, J=9.4 Hz, 1H), 8.14 (d, J=9.4 Hz, 1H), 8.34 (s, 1H), 8.43 (s, 1H), 8.89 (s, 1H), 9.92 (s, 1H), 10.95 (s, 1H).

Aufarbeitung

  1. customThe mixture was carefully evacuated
  2. customThe mixture was carefully evacuated
  3. temperatureto cool to rt
  4. customThe mixture was carefully evacuated
  5. customAgain, the mixture was carefully evacuated
  6. stirringwas stirred at 90° C. for 1 h
  7. temperatureThe reaction mixture was cooled to rt
  8. concentrationconcentrated in vacuo
  9. filtrationThe solution was filtered
  10. customThe filtercake was isolated
  11. waitto stand for 30 minutes
  12. filtrationfiltered
  13. washThe filtercake was washed with water
  14. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a3a84b961f614fad95a5afa31c78b5c5
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07820665B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion