Reaktion #1109644

ord-91dd31c9c4c443ac8a46a0e4a9270759

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter complete addition
  2. 2
    SonstigeVolatiles were evaporated under reduced pressure

Vorschrift

To a stirred solution of 2-bromo-5-iodobenzoic acid (150 g, 458 mmol) in dichloromethane (1500 ml) was added DMF (2.0 ml) followed by oxalylchloride (58.2 ml, 688 mmol) at 0° C. in drop wise fashion over the period of 30 min. After complete addition, the reaction mixture was stirred at room temperature for 3 h. Volatiles were evaporated under reduced pressure to give 2-bromo-5-iodo-benzoyl chloride (−158 g). The crude product was used for the next step immediately. (Note: The product should not be exposed to air).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08722633B2uspto-grants-2014_05