反应详情

温度

200 °C

A mixture of 1.42 g (10 mmol) phosphorus pentoxide, 1.38 g (10 mmol) triethylamine hydrochloride, and 1.46 g (10 mmol) 3-chloro-4-fluoroaniline is heated and stirred in a nitrogen atmosphere at 200° C. until a homogeneous melt has formed. To the melt, 0.593 g (2.5 mmol) 4-(4-pyridylmethyl)-1(2H)-phthalazinone is added and the reaction mixture stirred for a further 3 h at 200° C. After cooling to RT, the hyalinocrystalline reaction mixture is distributed between 150 ml dichloromethane and a mixture of 10 ml water and 20 ml 2N sodium hydroxide solution with intensive stirring and sonication. The organic phase washed with water and dried over sodium sulfate is concentrated by evaporation and the residue recrystallized from acetate. Title compound is obtained after a second recrystallization from methanol/water and drying under HV (8 h at 100° C.); m.p. 185-187° C.; ESI-MS: (M+H)+=365.

1. temperatureis heated
2. customhas formed
3. stirringthe reaction mixture stirred for a further 3 h at 200° C
4. temperatureAfter cooling to RT
5. customthe hyalinocrystalline reaction mixture
6. stirringwith intensive stirring
7. customsonication
8. washThe organic phase washed with water
9. dry with materialdried over sodium sulfate
10. concentrationis concentrated by evaporation
11. customthe residue recrystallized from acetate