反応 #1106678
ord-bf290e4dd92b40a5a8f798b219c541fd
反応方程式
((3,4-Dihydro-2H-benzo[b][1,4]dioxepin-3-yl)methyl)amine
sulfamide
Chloroform
→
title compound
((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温度heated
- 2温度to reflux overnight
- 3その他the precipitate was removed by filtration
- 4濃縮The filtrate was concentrated under vacuum
- 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.