反应详情

A solution of 10.0 g (29.66 mmol) of N-{1-[3-(4-bromophenyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl} from example 7A in 340 ml of 1,2-dichloroethane is treated with 13.64 g (8.30 ml, 88.98 mmol) of phosphoryl chloride. The mixture is boiled under reflux for 15 h. After cooling, the solvent is removed. The residue is stirred with diethyl ether and filtered off with suction. The crystals are stirred for 1 h with 150 ml of saturated aqueous sodium hydrogencarbonate solution, and subsequently diluted with 100 ml of water. After 30 min, the solid is filtered off with suction, washed well with water and rewashed with petroleum ether.

1. temperatureunder reflux for 15 h
2. temperatureAfter cooling
3. customthe solvent is removed
4. filtrationfiltered off with suction
5. stirringThe crystals are stirred for 1 h with 150 ml of saturated aqueous sodium hydrogencarbonate solution
6. additionsubsequently diluted with 100 ml of water
7. filtrationthe solid is filtered off with suction
8. washwashed well with water