반응 #156647

반응 방정식

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

용매

acetonitrile

water

반응 조건

후처리

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

실험 절차

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+).

출처