تفاعل #156647

معادلة التفاعل

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

المذيبات

acetonitrile

water

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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+).

المصدر