反应详情

温度

150 °C

1,2-Dimethylpiperazine (2.284 g, 20.00 mmol) and ethyl 4-fluorobenzoate (1.467 mL, 10 mmol) were dissolved in DMA (12 mL) and sealed in a microwave tube. The reaction was heated to 150° C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction mixture was heated for a further 30 mins at 150° C. and cooled to room temperature. The reaction mixture was evaporated and the crude product was purified by silica column chromatography, eluting with 5% MeOH in DCM with 0.1% 0.880 ammonia. Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.853 g, 32.5%) as a colourless waxy solid.

1. customsealed in a microwave tube
2. temperaturecooled to room temperature
3. temperatureThe reaction mixture was heated for a further 30 mins at 150° C.
4. temperaturecooled to room temperature
5. customThe reaction mixture was evaporated
6. customthe crude product was purified by silica column chromatography
7. washeluting with 5% MeOH in DCM with 0.1% 0.880 ammonia
8. customPure fractions were evaporated to dryness