Reaktion #65462

ord-2e7de4a67f654e6289e33cb572b49a01

Reaktionsgleichung

Cc1ccc(C(=O)O)cc1
ρ-toluic acid
O=C(Cl)C(=O)Cl
oxalyl chloride
Cc1ccc(C(=O)Cl)cc1
4-methylbenzoyl chloride

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe ice bath was removed
  2. 2
    SonstigeThe solvent was removed by rotary vacuum evaporation
  3. 3
    Sonstigewas pumped down under high vacuum overnight

Vorschrift

Meanwhile, the 4-methylbenzoyl chloride acylating agent was prepared by suspending 3.314 g (24.3 mmol) of ρ-toluic acid in 200 ml benzene. To this solution was added 2.0 equiv. (4.25 ml) of oxalyl chloride, dropwise via a pressure-equalizing dropping funnel at O° C. DMF (2-3 drops) was added to the reaction mixture catalytically and the ice bath was removed. The progress of the reaction was monitored via infrared spectroscopy. The solvent was removed by rotary vacuum evaporation and the residual oil was pumped down under high vacuum overnight.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420134uspto-grants-1995_05