反応 #444877

ord-7903e75866d04d5fb98f14728c9684aa

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwere added
  2. 2
    その他were pumped in over 8 hours at 60° C
  3. 3
    workup.ADDITIONAfter addition
  4. 4
    workup.DISTILLATIONThe product was then distilled

実験手順

268 g of 2,3,4,5-tetrafluorobenzotrichloride were placed in a stirred apparatus and 5.3 [lacuna] of iron(III) chloride were added, 45 g of formic acid (98-100%) were pumped in over 8 hours at 60° C. Vigorous gas development (carbon monoxide, hydrogen chloride) began immediately. The gas stream was fed to an absorption tower via a cooler. After addition was complete, the mixture was stirred until the end of gas development. The product was then distilled. 195 g of 2,3,4,5-tetrafluorobenzoyl chloride were obtained (91.5% of theory); b.p.: 70°-72° C./20 mbar, nD25 : 1.4773.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05840975uspto-grants-1998_11