反应详情

To a mixture of 11.80 g. of sodium hydride (61.14% oil dispersion) and 26.0 g. of 3,6-acridinediol sulfate (2:1) is added 250 ml. of dry N,N-dimethylformamide. The mixture is stirred at room temperature for 1.5 hours, then 49.8 g. of 3-chloropropyl-p-toluene sulfonate are added. This mixture is stirred at room temperature for 3 hours and 20 minutes, then at 50° C. for 2 hours. The volatile materials are removed under reduced pressure at 35°-40° C. and the residue is quenched with 1200 ml. of ice-cold saturated aqueous sodium bicarbonate solution. The resulting tan crystals are collected and dissolved in 500 ml. of chloroform. A 30 ml. portion of 6 N hydrochloric acid in isopropanol is added and the mixture is diluted with ether. The solid is collected and recrystallized from ether, giving the desired product as tan crystals, m.p. 211°-213° C.

1. additionTo a mixture of 11.80 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. additionportion of 6 N hydrochloric acid in isopropanol is added
9. additionthe mixture is diluted with ether
10. customThe solid is collected
11. customrecrystallized from ether