反应详情

In 20 ml of toluene, 2.0 g of 5-ethyl-2-imino-3-(2'-cyanobiphenyl-4-yl)methyl-1,3,4-thiadiazoline.hydrobromide and 1.1 g of trimethyltin azide were suspended, followed by heating under reflux for 6 hours. After cooling, the reaction mixture was subjected to column chromatography on a silica gel and eluted using chloroform:methanol (20:1)→chloroform:methanol:acetic acid (20:10:1). The eluate fraction thus obtained were then distilled off under reduced pressure. To the residue, 40 ml of 2N sodium hydroxide and 40 ml of ethyl acetate were added. The aqueous layer so obtained was neutralized with 12N hydrochloric acid and powders so precipitated were collected by filtration. The powders were washed successively with water, ethanol and then diethyl ether and then dried, whereby 56 mg of the title compound was obtained.

1. temperatureby heating
2. temperatureunder reflux for 6 hours
3. temperatureAfter cooling
4. washeluted
5. customThe eluate fraction thus obtained
6. distillationwere then distilled off under reduced pressure
7. additionTo the residue, 40 ml of 2N sodium hydroxide and 40 ml of ethyl acetate were added
8. customThe aqueous layer so obtained
9. customso precipitated
10. filtrationwere collected by filtration
11. washThe powders were washed successively with water, ethanol
12. dry with materialdiethyl ether and then dried