تفاعل #1106678

ord-bf290e4dd92b40a5a8f798b219c541fd

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةto reflux overnight
  3. 3
    أخرىthe precipitate was removed by filtration
  4. 4
    تركيزThe filtrate was concentrated under vacuum
  5. 5
    أخرىpurified by chromatography (2% to 8% acetone in dichloromethane)

الإجراء التجريبي

((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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08716231B2uspto-grants-2014_05