反応 #59677

ord-f706d26ebb73471d909c51f1695ddd4a

反応条件

温度
61°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was removed in vacuo and excess thionyl chloride
  2. 2
    その他removed
  3. 3
    その他by azeotroping with toluene (3×30 ml)

実験手順

Thionyl chloride (8.2 ml, 112.5 mmol) was added to a mixture of 3-iodo-4-methylbenzoic acid (18.5 g, 75 mmol) in chloroform (100 ml) and heated at 61° C. for 16 hours. The solvent was removed in vacuo and excess thionyl chloride removed by azeotroping with toluene (3×30 ml). The desired product was formed as a beige solid (19.5 g 93%) and used in subsequent reactions without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07425555B2uspto-grants-2008_09