Reaktion #45101

Reaktionsgleichung

Ethyl 4-fluorobenzoate

1-cyclobutylpiperazine

potassium carbonate

→

ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate

Ausbeute 33.0%

Lösungsmittel

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated to dryness
2. 2
   SonstigeThe residue was triturated with diethyl ether
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated
5. 5
   Sonstigethe crude product was purified by silica column chromatography
6. 6
   Wascheneluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM
7. 7
   SonstigePure fractions were evaporated to dryness

Vorschrift

Ethyl 4-fluorobenzoate (0.753 g, 4.48 mmol) was added to a solution of 1-cyclobutylpiperazine (0.571 g, 4.07 mmol) and potassium carbonate (0.563 g, 4.07 mmol) in DMSO (8 mL) under nitrogen. The resulting solution was stirred at 100° C. for 18 h and evaporated to dryness. The residue was triturated with diethyl ether, filtered, and evaporated and the crude product was purified by silica column chromatography, eluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate (0.387 g, 32.9%) as a white solid.

Quelle