反应详情

A mixture of 1,2-dibenzoyl-1H-1,2,5-triazepine (2.0 g), 4-vinylpyridine (1.42 g) and p-toluenesulfonic acid (1.21 g) in methanol (70 ml) was stirred and heated at 60° under a nitrogen atmosphere for 3 days. The foam, obtained after evaporation of the solvent, was mixed with dichloromethane and 10% sodium carbonate solution. The organic phase was washed with water until neutral washings were obtained and dried (Na2SO4). Evaporation of the solvent gave a foam, 2.25 g. The crude product was chromatographed on a column of silica gel; elution with ethanol-ethyl acetate-dichloromethane (1:4:5) giving a major component. A hydrochloride salt, 1/3 hydrate of the titled compound was formed in ethanol; wt. 1.2 g (38%), mp 247° dec.

1. temperatureheated at 60° under a nitrogen atmosphere for 3 days
2. customThe foam, obtained
3. customafter evaporation of the solvent
4. additionwas mixed with dichloromethane and 10% sodium carbonate solution
5. washThe organic phase was washed with water until neutral washings
6. customwere obtained
7. dry with materialdried (Na2SO4)
8. customEvaporation of the solvent
9. customgave a foam, 2.25 g
10. customThe crude product was chromatographed on a column of silica gel
11. washelution with ethanol-ethyl acetate-dichloromethane (1:4:5)
12. customgiving a major component