Reaktion #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

Reaktionsgleichung

NCC1COc2ccccc2OC1
((3,4-Dihydro-2H-benzo[b][1,4]dioxepin-3-yl)methyl)amine
NS(N)(=O)=O
sulfamide
ClC(Cl)Cl
Chloroform
NS(=O)(=O)NCC1COc2ccccc2OC1
title compound
NS(=O)(=O)NCC1COc2ccccc2OC1
((3,4-Dihydro-2H-benzo[b][1,4]dioxepin-3-yl)methyl)sulfamide

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturto reflux overnight
  3. 3
    Sonstigethe precipitate was removed by filtration
  4. 4
    EinengenThe filtrate was concentrated under vacuum
  5. 5
    Sonstigepurified by chromatography (2% to 8% acetone in dichloromethane)

Vorschrift

((3,4-Dihydro-2H-benzo[b][1,4]dioxepin-3-yl)methyl)amine (2.90 g, 16.2 mmol) and sulfamide (3.11 g, 32.4 mmol) were combined in dry dioxane (60 ml) and heated to reflux overnight. Chloroform was added and the precipitate was removed by filtration. The filtrate was concentrated under vacuum and purified by chromatography (2% to 8% acetone in dichloromethane) to yield the title compound as an off-white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08716231B2uspto-grants-2014_05