Reaktion #2475537

Reaktionsgleichung

1,4-dioxa-spiro[4.5]decane-8-carbonitrile

hydroxylamine

→

product

N-Hydroxy-1,4-dioxa-spiro[4.5]decane-8-carboxamidine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   SonstigeAfter removal of organic solvent
3. 3
   Sonstigeby evaporation
4. 4
   workup.DISSOLUTIONthe residue was dissolved in water
5. 5
   Extraktionextracted with EtOAc
6. 6
   Trocknendried over Na2SO4
7. 7
   FiltrationFiltration and evaporation to dryness

Vorschrift

A mixture of 1,4-dioxa-spiro[4.5]decane-8-carbonitrile (0.40 g, 2.4 mmol, prepared according to the procedure from Tremblay, Maxime, PCT Int. Appl. (2007), WO 2007013848) and hydroxylamine (Aldrich, 50% in H2O, 0.7 mL, 9.6 mmol) in ethanol (1.5 mL) in a sealed tube was heated to 80° C. for 6 h. After removal of organic solvent by evaporation, the residue was dissolved in water, extracted with EtOAc and dried over Na2SO4. Filtration and evaporation to dryness gave the product as a white solid.

Quelle