Reaktion #675766

ord-383135e79a1244a8aff3053bb178f680

Lösungsmittel

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated in vacuo
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    Filtrationthe solid was filtered
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigedried in vacuo

Vorschrift

To a solution of N-[3-(trifluoromethyl)-1H-pyrazol-5-yl]acetamide (7.3 g, 38 mmol) in ethanol (120 mL) were added iodic acid (1.65 g, 9.4 mmol) and iodine (4.8 g, 18.9 mmol). The reaction was stirred for 3.25 h at 65° C. The reaction mixture was concentrated in vacuo and the residue was suspended in hot CH2Cl2 (150 ml) with stirring, the solid was filtered and resuspended in hot CH2Cl2 (100 ml) filtered and dried in vacuo to provide the title compound as a white solid (8.9 g) which was used in the subsequent step.

Quelle

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