反应详情

温度

50 °C

To a suspension of tert-butyl chloroacetate (3.49 g, 34.9 mmol) and potassium carbonate (5.50 g, 39.8 mmol) in acetonitrile (300 mL) was added dropwise 1-methylpiperazine (5.00 g, 33.2 mmol), and the mixture was stirred with heating at 50° C. for 16 hr. The reaction mixture was cooled to room temperature, the insoluble material was filtered off, and the filtrate was concentrated. Water (150 mL) was added to the obtained residue, and the mixture was extracted with ethyl acetate (300 mL). The organic layer was washed with water (150 mL) and saturated brine (150 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (5.63 g, 79%) as a pale-yellow oil. The compound was used for the next reaction without further purification operation.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationthe insoluble material was filtered off
3. concentrationthe filtrate was concentrated
4. additionWater (150 mL) was added to the obtained residue
5. extractionthe mixture was extracted with ethyl acetate (300 mL)
6. washThe organic layer was washed with water (150 mL) and saturated brine (150 mL)
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationThe insoluble material was filtered off
9. concentrationthe filtrate was concentrated