反应详情

温度

0 °C

To a solution of S-(−)-1-phenyl ethylamine (15.75 g, 130 mmol) in 150 mL of DMF at 0° C. is added K2CO3 (53.9 g, 390 mmol) in small portions. After stirring at 0° C. for 10 min, 4-bromobutene (13.5 g, 100 mmol) is added dropwise and followed by Nal (58.5 g, 390 mmol) in small portions. The reaction mixture, a white suspension, is heated to 95° C. and stirred overnight/16 hrs. The solution is cooled to RT and diluted with 200 mL of ether, and washed with 3×100 ml of water. The organic layer is dried over Na2SO4 and concentrated. The crude product is purified by distillation (65˜70° C. under high vacuum) to yield a colorless liquid(13.5 g, 76.7%). (NMR and MS data confirmed, U-4117-28-23).

1. temperatureThe reaction mixture, a white suspension, is heated to 95° C.
2. stirringstirred overnight/16 hrs
3. temperatureThe solution is cooled to RT
4. washwashed with 3×100 ml of water
5. dry with materialThe organic layer is dried over Na2SO4
6. concentrationconcentrated
7. distillationThe crude product is purified by distillation (65˜70° C. under high vacuum)