Реакция #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated
  2. 2
    Температураto reflux overnight
  3. 3
    Другоеthe precipitate was removed by filtration
  4. 4
    КонцентрированиеThe filtrate was concentrated under vacuum
  5. 5
    Другоеpurified by chromatography (2% to 8% acetone in dichloromethane)

Методика

((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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08716231B2uspto-grants-2014_05