Reaktion #675796

ord-e0a58e14d88c4772b337fbad60fd3375

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    EinengenThe reaction mixture was concentrated in vacuo
  3. 3
    Sonstigepartitioned between CH2Cl2 and 2 M Na2S2O3 aq. solution
  4. 4
    SonstigeThe layers were separated
  5. 5
    Waschenthe organic washed with brine
  6. 6
    Trocknendried (MgSO4)
  7. 7
    Einengenconcentrated in vacuo

Vorschrift

A suspension of N-[3-(3-fluorophenyl)-1H-pyrazol-5-yl]acetamide (7.6 g, 34.7 mmol), iodic acid (1.5 g, 8.5 mmol) and iodine (4.4 g, 17.3 mmol) in ethanol (200 mL) was heated at 60° C. for 1 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and partitioned between CH2Cl2 and 2 M Na2S2O3 aq. solution. The layers were separated and the organic washed with brine, dried (MgSO4), and concentrated in vacuo to provide the title compound as a solid (10.8 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09227976B2uspto-grants-2016_01