Reacción #327491

Ecuación de reacción

4,4-Difluoropiperidine hydrochloride

1

9-oxo-9H-indeno[1,2-b]pyrazine-2,3-dicarbonitrile

→

8

Rendimiento 95.0%

3-(4,4-difluoro-piperidin-1-yl)-9-oxo-9H-indeno[1,2-b]-pyrazine-2-carbonitrile

Rendimiento 95.0%

Disolventes

NaOH

THF

Condiciones de reacción

Tratamiento posterior

1. 1
   Extracciónextracted with CH2Cl2 (2×5 ml)
2. 2
   SecadoOrganic phase was dried over Na2SO4
3. 3
   Filtraciónfiltered
4. 4
   Otroevaporated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in THF (2 ml)
6. 6
   OtroThe solvent was evaporated
7. 7
   Lavadothe crude solid washed with EtOH
8. 8
   Otrodried under vacuum

Procedimiento

4,4-Difluoropiperidine hydrochloride (249 mg, 1.58 mmol) was dissolved in 1N NaOH (5 ml) and extracted with CH2Cl2 (2×5 ml). Organic phase was dried over Na2SO4, filtered and evaporated. The residue was dissolved in THF (2 ml) and this solution was added to a solution of 1 (185 mg, 0.79 mmol) in THF (2 ml); the mixture was stirred at room temperature for 48 hours. The solvent was evaporated, the crude solid washed with EtOH and dried under vacuum, affording 8 (245 mg, 95%) as yellow-brown solid.

Fuente