반응 #46113

ord-8df3b2af4ad44a3c9cd5221054a83a8f

용매

반응 조건

온도
105°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent and the excess of amine are removed by distillation under reduced pressure
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in methanol (20 mL)
  3. 3
    온도The methanolic solution is cooled on an ice bath
  4. 4
    workup.ADDITIONwater (60 mL) is added

실험 절차

A solution of 4,5-dichloro-2-fluorobenzenesulphonamide (3 g) in dioxane (30 mL) to which cyclopropylamine (3 mL) has been added is heated at 100-110° C. in a hermetically closed vessel for 24 hours. The solvent and the excess of amine are removed by distillation under reduced pressure and the residue is dissolved in methanol (20 mL). The methanolic solution is cooled on an ice bath, and water (60 mL) is added. The precipitate obtained (the title product) is collected by filtration, washed with water and dried. It is used in the following Step without being otherwise purified.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741320B2uspto-grants-2010_06