反应详情

温度

90 °C

63.3 g (0.045 mol) of the 1,5,8,12,15,18,21-Heptakis(p-tolylsulfonyl)-1,5,8,12,15,18,21-heptaazacyclotricosane was mixed with 300 ml of 98% sulfuric acid and 8 ml of water, and then the mixed solution was heated at a temperature of 90° C. for 3 days and then cooled. The mixed solution was added to 2000 ml of diethylether and then diethylether was subjected to decanting, and the residual was dissolved in 200 ml of water. A pH of the resultant solution was controlled to be pH 13 by using a NaOH aqueous solution, and the solution was filtered and extracted with ethanol. The ethanol used was evaporated from the extraction product and impurities were removed therefrom under vacuum conditions according to a kugelrohr distillation method to produce 8 g of 1,5,8,12,15,18,21-heptaazacyclotricosane.

1. temperaturecooled
2. customto decanting
3. dissolutionthe residual was dissolved in 200 ml of water
4. filtrationthe solution was filtered
5. extractionextracted with ethanol
6. customThe ethanol used was evaporated from the extraction product and impurities
7. customwere removed
8. distillationunder vacuum conditions according to a kugelrohr distillation method