Reaktion #441347

ord-3ef1a7dde81643968328fe800d633c49

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered
  2. 2
    Einengenconcentrated
  3. 3
    SonstigeRecrystallisation from hot ethyl acetate

Vorschrift

10% Palladium on carbon (100 mg) was added to a stirred slurry of 3-ethyl-2-(2-methoxyethyl)-4-nitro-pyrazole-5-carboxamide (5 g, 20.77 mmol) in ethanol (100 mL) and the mixture stirred in a pressure vessel under a hydrogen atmosphere (344.7 kPa (50 psi)) at room temperature for 6 h. The mixture was filtered and concentrated. Recrystallisation from hot ethyl acetate gave the product as white crystals (3.5 g). The mother liquor was concentrated to give a further 1.5 g of product as a grey powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06756373B1uspto-grants-2004_06