反応 #1483254

ord-57ba6ca22e26401894c70e6b4a637b3b

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwere added dropwise at 5° C.
  2. 2
    その他Subsequently, the cooling was removed
  3. 3
    workup.STIRRINGthe mixture was stirred at room temperature for a further 16 hours
  4. 4
    ろ過Under argon, the solid pyridinium hydrochloride was then filtered off
  5. 5
    濃縮the solution was concentrated

実験手順

10 g of p-toluamide were suspended in 100 ml of ether and 12.5 ml of pyridine under argon. The 5.8 ml of thionyl chloride dissolved in 10 ml of ether were added dropwise at 5° C. and the mixture was stirred for a further 5 minutes. Subsequently, the cooling was removed and the mixture was stirred at room temperature for a further 16 hours. Under argon, the solid pyridinium hydrochloride was then filtered off, and then the solution was concentrated. The residue was used without further workup.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08901114B2uspto-grants-2014_12