Reaction #156647

Reaction equation

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

Solvents

acetonitrile

water

Conditions

Workup

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

Procedure

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+).

Source