Reaktion #156647

Reaktionsgleichung

Potassium carbonate

3,4-difluoronitrobenzene

1,4-dioxa-7-aza-spiro[4.4]nonane

Ethyl acetate

→

7-(2-Fluoro-4-nitro-phenyl)-1,4-dioxa-7-aza-spiro[4.4]nonane

Lösungsmittel

acetonitrile

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe aqueous phase was extracted several times with ethyl acetate
2. 2
   Trocknendried over sodium sulfate
3. 3
   Sonstigethe solvent was removed in vacuum
4. 4
   SonstigeIn this way the product was obtained with molecular weight 268.24 (C12H13FN2O4)

Vorschrift

Potassium carbonate (6.9 g) was added to a mixture of 3,4-difluoronitrobenzene (8.0 g) and 1,4-dioxa-7-aza-spiro[4.4]nonane (12.9 g) in acetonitrile (34.6 mL) and the reaction mixture was heated for 2 h at 75° C. Ethyl acetate and water were added to the reaction mixture. The aqueous phase was extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 268.24 (C12H13FN2O4); MS (ESI): 269 (M+H+).

Quelle