Reaction #1106678

Reaction equation

((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

Solvents

dioxane

Conditions

Workup

1. 1
   Temperatureheated
2. 2
   Temperatureto reflux overnight
3. 3
   Otherthe precipitate was removed by filtration
4. 4
   ConcentrationThe filtrate was concentrated under vacuum
5. 5
   Otherpurified by chromatography (2% to 8% acetone in dichloromethane)

Procedure

((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.

Source