반응 #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도to reflux overnight
  3. 3
    기타the precipitate was removed by filtration
  4. 4
    농축The filtrate was concentrated under vacuum
  5. 5
    기타purified by chromatography (2% to 8% acetone in dichloromethane)

실험 절차

((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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08716231B2uspto-grants-2014_05