Reaktion #540521

Reaktionsgleichung

Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine

sulfamide

→

title compound

N-(2,3-Dihydro-benzo[1.4]dioxin-2-ylmethyl)-sulfamide

Lösungsmittel

1,4 dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 2 h
2. 2
   Filtrationa small amount of solid was filtered
3. 3
   SonstigeThe filtrate was evaporated in vacuo
4. 4
   Sonstigethe residue was purified
5. 5
   Sonstigeto yield a white solid
6. 6
   SonstigeThe solid was recrystallized from DCM

Vorschrift

Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine (4.4 g, 26 mmol) and sulfamide (5.1 g, 53 mmol) were combined in 1,4 dioxane (100 mL) and refluxed for 2 h. The reaction was cooled to room temperature and a small amount of solid was filtered and discarded. The filtrate was evaporated in vacuo and the residue was purified using flash column chromatography (DCM:Methanol—10:1) to yield a white solid. The solid was recrystallized from DCM to yield the title compound as a white solid.

Quelle