Methyl iodide → HCID 67448855, Verbindung

HRID 68670Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 68670
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([SH:17])=[N:7][N:8]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1.[C:18]([O-])([O-])=O.[Cs+].[Cs+].IC>CC#N>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([S:17][CH3:18])=[N:7][N:8]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178527921HCID 178527921, Verbindung

Produkt 1

HCID 67448855HCID 67448855, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Into a 500-mL 3-necked round-bottom flask, was placed a solution of 6-bromo-1-phenyl-1H-indazole-3-thiol (24 g, 78.69 mmol, 1.00 equiv) in CH3CN (200 mL), Cs2CO3 (28.8 g, 88.34 mmol, 1.12 equiv). To the resulting mixture as then added iodomethane (12.6 g, 88.73 mmol, 1.13 equiv) dropwise with stirring at room temperature. The resulting solution was stirred for 60 min at room temperature. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:100) to yield 6-bromo-3-(methylthio)-1-phenyl-1H-indazole as a yellow solid. MS: 328 (MH+).

Aufarbeitung

  1. customInto a 500-mL 3-necked round-bottom flask, was placed
  2. filtrationThe solids were filtered out
  3. concentrationThe resulting mixture was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-e24347ed936b42c58c2bf9e6010016e9
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822447B2

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