反应详情

A vigorously stirred solution 13.15 g (0.05 mole) of o-xylylene dibromide and 7.3 g (0.05 mole) of t-butyl 2-methylcarbazate in 25 ml of dimethylformamide was warmed to 50° and 14 ml of triethylamine was added during 5-8 minutes while maintaining the temperature at 50°-60°. After complete addition the reaction mixture was stirred at room temperature for 3 hrs. and diluted with 100 ml of water. After stirring for 1 hr the mixture was extracted with ethyl acetate. The organic phase was separated and dried. Filtration and evaporation gave a gummy solid which was used without further purification. The IR and NMR of the material were consistent with the proposed structure.

1. temperaturewhile maintaining the temperature at 50°-60°
2. additionAfter complete addition the reaction mixture
3. stirringAfter stirring for 1 hr the mixture
4. extractionwas extracted with ethyl acetate
5. customThe organic phase was separated
6. customdried
7. filtrationFiltration and evaporation
8. customgave a gummy solid which
9. customwas used without further purification