Reaktion #333824

ord-ba94e7cba97045b59f9c65c67025b88a

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
30°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeReaction
  2. 2
    Sonstigequenched with water, product
  3. 3
    Extraktionwas extracted with ethyl acetate (150 mL), organic phase
  4. 4
    Waschenwashed with water (3×10 mL), brine (2×10 mL)
  5. 5
    Trocknendried over Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated

Vorschrift

A mixture of 6-chloro-1H-indazole (2 g, 13.1 mmol), KOH (2.2 g, 39.3 mmol) and I2 (6.6 g, 26.2 mmol) in dry DMF (20 mL) was heated to 30° C. for 16 hours. Reaction quenched with water, product was extracted with ethyl acetate (150 mL), organic phase washed with water (3×10 mL), brine (2×10 mL) and dried over Na2SO4, then filtered and concentrated to afford 6-chloro-3-iodo-1H-indazole (3.0 g, 83%) as a yellow solid. LCMS: (M+H)+=279.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08658646B2uspto-grants-2014_02