反応 #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated
  2. 2
    温度to reflux overnight
  3. 3
    その他the precipitate was removed by filtration
  4. 4
    濃縮The filtrate was concentrated under vacuum
  5. 5
    その他purified by chromatography (2% to 8% acetone in dichloromethane)

実験手順

((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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08716231B2uspto-grants-2014_05