Реакция #46113

ord-8df3b2af4ad44a3c9cd5221054a83a8f

Уравнение реакции

NS(=O)(=O)c1cc(Cl)c(Cl)cc1F
4,5-dichloro-2-fluorobenzenesulphonamide
NC1CC1
cyclopropylamine
NS(=O)(=O)c1cc(Cl)c(Cl)cc1NC1CC1
title product
NS(=O)(=O)c1cc(Cl)c(Cl)cc1NC1CC1
4,5-dichloro-2-cyclopropylaminobenzenesulphonamide

Реагенты

Нет

Растворители

Условия реакции

Температура
105°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe 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
    ТемператураThe methanolic solution is cooled on an ice bath
  4. 4
    workup.ADDITIONwater (60 mL) is added

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07741320B2uspto-grants-2010_06