反应详情

4-(3-hydroxypropyl)piperazinylcarboxylic acid ethyl ester (14.06 g, 65.09 mmol), 10% sodium hydroxide aqueous solution (150 mL) and ethanol (150 mL) were placed in a 500 mL round bottom flask, heated for refluxing and stirred overnight. The reaction was cooled down to room temperature, distilled under a reduced pressure to remove the solvent to obtain a light yellow oily substance, which was added with 200 mL saturated saline, and the resulting mixture was extracted with dichloromethane (5×200 mL), dried (Na2SO4), filtered, concentrated to obtain a light yellow oily substance, 7.56 g, yield 80.7%, which was directly used in the next step of reaction.

1. temperatureheated
2. temperaturefor refluxing
3. distillationdistilled under a reduced pressure
4. customto remove the solvent
5. customto obtain a light yellow oily substance, which
6. additionwas added with 200 mL saturated saline
7. extractionthe resulting mixture was extracted with dichloromethane (5×200 mL)
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customto obtain a light yellow oily substance, 7.56 g, yield 80.7%, which
12. customwas directly used in the next step of reaction