反应详情

温度

50 °C

Propynylbromide (11.9 g.) was added to the sodium salt of N-(2-pyridyl)piperazine prepared from 16.3 g. of N-(2-pyridyl)piperazine and 4.8 g. of sodium hydride/50% mineral oil dispersion in 50 ml. of dry dimethylformamide. The mixture was stirred at 50° C. for 3 hours and then carefully poured into 3 volumes of cold water. This mixture was extracted with several portions of either and the combined ether extracts were washed twice with 10% aqueous hydrochloric acid. The acidic extract was made strongly alkaline by adding 40% aqueous sodium hydroxide under cooling. The mixture was then extracted several times with ether and the combined extracts were dried over magnesium sulfate. The latter was then removed by filtration, and the filtrate was evaporated to produce a brown oil. Distillation under reduced pressure gave N'-(2-pyridyl)-N-(2-propynyl)piperazine, b.p. 153°-4° C./3.5 mm, as a yellow oil which showed the expected NMR and IR spectra.

1. customprepared from 16.3 g
2. extractionThis mixture was extracted with several portions of either and the combined ether extracts
3. washwere washed twice with 10% aqueous hydrochloric acid
4. extractionThe acidic extract
5. additionby adding 40% aqueous sodium hydroxide
6. temperatureunder cooling
7. extractionThe mixture was then extracted several times with ether
8. dry with materialthe combined extracts were dried over magnesium sulfate
9. customThe latter was then removed by filtration
10. customthe filtrate was evaporated
11. customto produce a brown oil
12. distillationDistillation under reduced pressure