Reaktion #45042

Reaktionsgleichung

2,6-Dimethylpiperazine

ethyl 4-fluorobenzoate

→

ethyl 4-(3,5-dimethylpiperazin-1-yl)benzoate

Ausbeute 76.0%

Lösungsmittel

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled
2. 2
   Sonstigethe solvent was evaporated
3. 3
   SonstigeThe crude product was purified by silica column chromatography
4. 4
   Wascheneluting with 10% methanol in dichloromethane containing 1% 0.880 ammonia
5. 5
   SonstigePure fractions were evaporated to dryness

Vorschrift

2,6-Dimethylpiperazine(3.43 g, 30.00 mmol) was added to ethyl 4-fluorobenzoate (1.101 mL, 7.5 mmol), in DMSO (10 mL) warmed to 120° C. under nitrogen. The resulting solution was stirred at 120° C. for 20 h. The reaction mixture was cooled and the solvent was evaporated. The crude product was purified by silica column chromatography, eluting with 10% methanol in dichloromethane containing 1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,5-dimethylpiperazin-1-yl)benzoate (1.490 g, 76%) as a colourless solid.

Quelle