반응 #45059

반응 방정식

Ethyl 4-fluorobenzoate

1-cyclobutylpiperazine

→

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

수율 11.3%

용매

DMA

반응 조건

후처리

1. 1
   기타sealed into a microwave tube
2. 2
   온도cooled to room temperature
3. 3
   기타The reaction mixture was evaporated to dryness
4. 4
   기타the crude product purified by silica column chromatography
5. 5
   세척eluting with a gradient of 0-2.5% MeOH in DCM
6. 6
   기타Pure fractions were evaporated to dryness

실험 절차

Ethyl 4-fluorobenzoate (0.225 mL, 1.53 mmol) and 1-cyclobutylpiperazine (0.430 g, 3.07 mmol) were taken up in DMA (3 mL) and sealed into a microwave tube. The reaction was heated to 150° C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction was not complete, so it was reheated at 150° C. for a further 1 h. The reaction mixture was evaporated to dryness and the crude product purified by silica column chromatography, eluting with a gradient of 0-2.5% MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-cyclobutylpiperazin-1-yl)benzoate (0.050 g, 11.31%) as a yellow solid.

출처