Reacción #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

Ecuación de reacción

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

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturato reflux overnight
  3. 3
    Otrothe precipitate was removed by filtration
  4. 4
    ConcentraciónThe filtrate was concentrated under vacuum
  5. 5
    Otropurified by chromatography (2% to 8% acetone in dichloromethane)

Procedimiento

((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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08716231B2uspto-grants-2014_05