反应详情

温度

80 °C

To the solution of bis(2-chloroethyl)-(3-phenylpropyl)ammonium chloride (1.78 g, 6 mmol) and 2-(3-methylphenyl)ethanamine (0.811 g, 6 mmol) in 8 mL of DMF is added anhydrous potassium carbonate (2.48 g, 18 mmol) and sodium iodide (1.80 g, 12 mmol) successively. The reaction mixture is then stirred at 80° C. for 4 hours and then cooled to ambient temperature. Water and ethyl acetate are then added to the resultant reaction mixture. The organic layer is separated, washed 3 times with water and once with brine, dried over anhydrous magnesium sulfate, and concentrated. The residue is dissolved in ethanol. To this solution is added 6 N hydrochloric acid drop wise with cooling until pH 3. The resulting solution is maintained at 4° C. overnight. The resultant crystals are collected by filtration and washed with ether to give 97 mg of the title compound (5%).

1. temperaturecooled to ambient temperature
2. customreaction mixture
3. customThe organic layer is separated
4. washwashed 3 times with water
5. dry with materialonce with brine, dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. dissolutionThe residue is dissolved in ethanol
8. additionTo this solution is added 6 N hydrochloric acid
9. temperaturewith cooling until pH 3
10. temperatureThe resulting solution is maintained at 4° C. overnight
11. filtrationThe resultant crystals are collected by filtration
12. washwashed with ether