Iodine → HCID 178455023, Verbindung

HRID 246718

Reaktionsgleichung

Reaktionsgleichung von HRID 246718
[Si:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][N:13]=[CH:12]2)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH-].[K+].[I:20]I>CS(C)=O>[Si:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][N:13]=[C:12]2[I:20])([C:4]([CH3:7])([CH3:5])[CH3:6])([CH3:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 807IodineHCID 14797Potassium HydroxideHCID 580425115-[[(1,1-Dimethylethyl)dimethylsilyl]oxy]-1H-indazole

Produkt 1

HCID 178455023HCID 178455023, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

To a stirred solution of 5-(tert-butyldimethylsilyloxy)-1H-indazole (5.3 g, 0.02 mol) in DMSO (50 mL) at 0° C., was added KOH (3.36 g, 0.06 mol) followed by iodine (10.2 g, 0.04 mol) portionwise. The mixture was stirred at room temperature for additional 10 minutes, then the reaction was quenched with 10% Na2S2O3 and diluted with water. The mixture was filtered and the filter cake was washed with water and dried to give 5-(tert-butyldimethylsilyloxy)-3-iodo-1H-indazole. The crude solid was used in the next step without purification. MS: (M+H)+=375.

Aufarbeitung

  1. customthe reaction was quenched with 10% Na2S2O3
  2. additiondiluted with water
  3. filtrationThe mixture was filtered
  4. washthe filter cake was washed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-141fc4217c0e4b0dbff96dcea8947c54
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658646B2

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