반응 #45101

반응 방정식

Ethyl 4-fluorobenzoate

1-cyclobutylpiperazine

potassium carbonate

→

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

수율 33.0%

용매

DMSO

반응 조건

후처리

1. 1
   기타evaporated to dryness
2. 2
   기타The residue was triturated with diethyl ether
3. 3
   여과filtered
4. 4
   기타evaporated
5. 5
   기타the crude product was purified by silica column chromatography
6. 6
   세척eluting with a gradient of 0 to 2.5% 2.5N MeOH in DCM
7. 7
   기타Pure fractions were evaporated to dryness

실험 절차

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.

출처