Iodine → HCID 178422150, Verbindung

HRID 1527305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1527305
[CH3:1][C:2]1[CH:3]=[C:4]2[CH:10]=[N:9][NH:8][C:5]2=[CH:6][N:7]=1.[I:11]I.[OH-].[K+]>CN(C=O)C.S([O-])([O-])(=O)=S.[Na+].[Na+].O>[I:11][C:10]1[C:4]2[C:5](=[CH:6][N:7]=[C:2]([CH3:1])[CH:3]=2)[NH:8][N:9]=1

Komponenten

7

Edukt 3

HCID 807IodineHCID 14797Potassium HydroxideHCID 126684875-methyl-1H-pyrazolo[3,4-c]pyridine

Produkt 1

HCID 178422150HCID 178422150, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 24477Sodium ThiosulfateLösungsmittel

Versuchsvorschrift

To a solution of 5-methyl-1H-pyrazolo[3,4-c]pyridine [76006-06-9] (1.00 g, 7.51 mmol) in DMF (15 mL) were added iodine (2.86 g, 11.3 mmol) and potassium hydroxide (1.05 g, 18.8 mmol). The reaction mixture was stirred at RT for 60 h. The mixture was diluted with 10% sodium thiosulfate and water, the resulting suspension was filtered. The solid was washed with water and then dried under vacuum. MS (LC/MS): 260.0 [M+H]+; tR (HPLC conditions k): 0.28 min.

Aufarbeitung

  1. filtrationthe resulting suspension was filtered
  2. washThe solid was washed with water
  3. customdried under vacuum
  4. custom0.28 min.

Quellen und Nachweise

ORD-Eintrag
ord-f50e95164ca641cda9cc78c5c70e8ef5
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085555B2

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