反应详情

温度

70 °C

A solution of 3-aminohomopiperidine (1.71 g, 15 mmol) in CH3CN (45 mL) was treated with p-chlorobenzyl chloride (463 mg, 2.9 mmol) and K2CO (828 g, 6 mmol) and heated to 70° C. for 9 h. The reaction mixture was cooled to 25° C. and concentrated to afford a yellow solid. The residue was partitioned between H2O (5 mL) and EtOAc (50 mL), and extracted with EtOAc (2×50 mL). The combined organic extracts were washed with brine (20 mL), dried (Na2SO4) and concentrated. The resulting yellow oil was purified by chromatography (SiO2, 5-20% CH3OH—CH2Cl2 gradient elution) to afford the desired product as a yellow oil (639 mg, 93%).

1. temperatureThe reaction mixture was cooled to 25° C.
2. concentrationconcentrated
3. customto afford a yellow solid
4. customThe residue was partitioned between H2O (5 mL) and EtOAc (50 mL)
5. extractionextracted with EtOAc (2×50 mL)
6. washThe combined organic extracts were washed with brine (20 mL)
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. customThe resulting yellow oil was purified by chromatography (SiO2, 5-20% CH3OH—CH2Cl2 gradient elution)