Reaktion #76768

ord-12e43ba8c0a54ca287305fcda8c0e43d

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to 0° C
  2. 2
    workup.STIRRINGlower, and the mixture was stirred at 10° C. or lower for 3 hours
  3. 3
    FiltrationThe precipitated crystals were collected by filtration
  4. 4
    Sonstigedried

Vorschrift

First, 50 g (0.61 mol) of sodium acetate and 41 g (0.14 mol) of 1,1-dibromo-3,3,3-trifluoroacetone were mixed with 500 ml of water, and the mixture was stirred at 80° C. for 30 minutes and then cooled to 0° C. Then, 45 g (0.14 mol) of 4-bromo-2-fluoro-5-isopropoxyphenylhydrazine hydrochloride was added at 10° C. or lower, and the mixture was stirred at 10° C. or lower for 3 hours. The precipitated crystals were collected by filtration and dried, which afforded 35 g (94.3 mmol) of 3,3,3-trifluoro-2-oxopropanal 1-(4-bromo-2-fluoro-5-isopropoxyphenylhydrazone).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06703503B2uspto-grants-2004_03