反应详情

A mixture of 29.25 g. (0.40 mole) isobutylamine and 48.82 g. (0.20 mole) 2-(methylthio)-2-imidazoline hydroiodide in 250 ml. abs. EtOH were refluxed for 2 hr. The mixture was concentrated in vacuo to a viscous oil, which was dissolved in 100 ml. abs. EtOH and added to a solution of 18.40 g. (0.80 mole) sodium and 22.62 g. (0.20 mole) ethyl cyanoacetate in 1200 ml. abs. EtOH. The mixture was refluxed for 3 hr., then concentrated in vacuo to a viscous oil. Water (400 ml.) was added and a white solid slowly crystallized. The solid was filtered and air-dried to yield 35.43 g. (86%), mp 235°-238° (two crops). Recrystallization from CH3CN gave white crystals, mp 230.5°-232.5° (corr.).

1. additionA mixture of 29.25 g
2. concentrationThe mixture was concentrated in vacuo to a viscous oil, which
3. dissolutionwas dissolved in 100 ml
4. additionEtOH and added to a solution of 18.40 g
5. temperatureThe mixture was refluxed for 3 hr
6. concentration, then concentrated in vacuo to a viscous oil
7. additionWater (400 ml.) was added
8. customa white solid slowly crystallized
9. filtrationThe solid was filtered
10. customair-dried
11. customto yield 35.43 g
12. customRecrystallization from CH3CN
13. customgave white crystals, mp 230.5°-232.5° (corr.)