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 6N 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 6N hydrochloric acid in isopropanol is added
9. additionthe mixture is diluted with ether
10. customThe solid is collected
11. customrecrystallized from ether