反应详情

To a mixture of 11.8 g. of sodium hydride (61.1% dispersion in oil) and 26.0 g. of 3,6-acridinediol is added 250 ml. of dimethylformamide. The mixture is stirred at room temperature for 1.5 hours, then 52.5 g. of 4-chlorobutyl-p-toluenesulfonate are added. This mixture is stirred at room temperature for 3 hours and 20 minutes and then at 50° C. for 2 hours. The volatile materials are removed under reduced pressure at 35°-40° C. The residue is quenched with 1200 ml. of ice-cold saturated aqueous sodium bicarbonate. The resulting tan crystals are collected and dissolved in 500 ml. of chloroform, 30 ml. of 6 N hydrochloric acid in isopropanol are added and the mixture is diluted with ether, giving the desired product as the hydrochloride salt.

1. additionTo a mixture of 11.8 g
2. stirringThis mixture is stirred at room temperature for 3 hours and 20 minutes
3. waitat 50° C. for 2 hours
4. customThe volatile materials are removed under reduced pressure at 35°-40° C
5. customThe residue is quenched with 1200 ml
6. customThe resulting tan crystals are collected
7. dissolutiondissolved in 500 ml
8. additionof 6 N hydrochloric acid in isopropanol are added
9. additionthe mixture is diluted with ether