反应详情

A mixture of sodium hydride (0.72 g) and 1-methyl-N5 -[3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1H-1,2,4-triazole-3,5-diamine (3.44 g) in dimethylformamide (50 ml) was heated under reflux for 8 h. The reaction mixture was cooled, poured onto water (300 ml) and extracted with ether. Evaporation of the organic extract gave a yellow oil, which was extracted with boiling cyclohexane (500 ml). As the cyclohexane extract was cooled a brown oil precipitated out. This oil was discarded and the supernatant solution was cooled to room temperature to give the title compound which was recrystallised from a mixture of ethyl acetate and light petroleum (b.p. 60°-80°) as a pale yellow solid (0.35 g) m.p. 68°-75° (decomposition). tlc, System C: Rf 0.6.

1. temperaturewas heated
2. temperatureunder reflux for 8 h
3. temperatureThe reaction mixture was cooled
4. additionpoured onto water (300 ml)
5. extractionextracted with ether
6. customEvaporation of the
7. extractionorganic extract
8. customgave a yellow oil, which
9. extractionwas extracted with boiling cyclohexane (500 ml)
10. extractionAs the cyclohexane extract
11. temperaturewas cooled a brown oil
12. customprecipitated out