반응 #78169

반응 방정식

carbonate

phosphorus pentoxide

triethylamine hydrochloride

4-aminobiphenyl

4-(4-pyridylmethyl)-1(2H)-phthalazinone

→

Title compound

1-(4-Phenylanilino)-4-(4-pyridylmethyl)phthalazine

용매

dichloromethane methanol

water

반응 조건

후처리

1. 1
   온도After cooling to RT
2. 2
   workup.STIRRINGwith intensive stirring
3. 3
   건조The organic phase dried over sodium sulfate
4. 4
   기타is evaporated under vacuum
5. 5
   기타the residue purified by means of flash chromatography on silica gel with particle size 0.04-0.06 mm

실험 절차

A mixture of 2.41 g (16.98 mmol) phosphorus pentoxide, 2.32 g (16.85 mmol) triethylamine hydrochloride, 3 g (17.73 mmol) 4-aminobiphenyl, and 1 g (4.21 mmol) 4-(4-pyridylmethyl)-1(2H)-phthalazinone is stirred for 20 h at 200° C. under a nitrogen atmosphere. After cooling to RT, the hyalinocrystalline melt is distributed between a dichloromethane/methanol mixture (99:1) and a mixture of water and saturated aqueous carbonate solution on (1:1) with intensive stirring and the use of an ultrasonic bath. The organic phase dried over sodium sulfate is evaporated under vacuum and the residue purified by means of flash chromatography on silica gel with particle size 0.04-0.06 mm, using a dichloromethane/methanol mixture (49:1). Title compound is obtained after evaporation of the product-containing fractions under vacuum and recrystallization of the residue from acetonitrile; m.p. 189-191 °C.; ESI-MS: (M+H)+=389.

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