Reaktion #540266

ord-14505f5a164b4ab4bc8ed155a593d42e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction mixture was evaporated to dryness at reduced pressure
  2. 2
    workup.ADDITIONThen toluene (100 mL) was added
  3. 3
    Einengenthe reaction mixture was concentrated again under vacuum

Vorschrift

To a 100 mL flask, 3-bromo-1-(3,5-dichloropyridin-2-yl)-1H-pyrazole-5-carboxylic acid (0.4 g, 1.2 mmol), dichloromethane (10 mL) and oxalyl dichloride (0.31 g, 2.4 mmol) were added. After five drops of N,N-dimethyl formamide was added, a large number of gas was released. After being stirred for 8 hours at room temperature, the reaction mixture was evaporated to dryness at reduced pressure. Then toluene (100 mL) was added, and the reaction mixture was concentrated again under vacuum to give the product (0.42 g) as green solid in 100% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08492409B2uspto-grants-2013_07