반응 #78190

반응 방정식

benzoyl chloride

aluminium chloride

1-(4-chloroanilino)phthalazine

trimethylsilyl cyanide

→

title compound

2-Benzoyl-4-(4-chloroanilino)-1,2-dihydrophthalazine-1-carbonitrile

용매

dichloromethane

water

반응 조건

후처리

1. 1
   여과filtered off
2. 2
   세척washed with water
3. 3
   기타dried
4. 4
   workup.ADDITIONMixing in 150 ml

실험 절차

Under N2 atmosphere, first 164 mg (1.2 mmol) anhydrous aluminium chloride is added to 12.6 g (49.3 mmol) 1-(4-chloroanilino)phthalazine in 90 ml dichloromethane, followed by 12.3 ml (98.6 mmol) trimethylsilyl cyanide. Finally, 11.5 ml (98.6 mmol) benzoyl chloride is added under ice cooling and stirred for 3 h at RT. The suspension is poured onto 0.6 ml water, filtered off, washed with water, and dried. Mixing in 150 ml boiling ethanol yields pure title compound: m.p.: 201-202° C.; Anal. calc.(C22H15N4ClO) C, 68.31%; H, 3.91%; N, 14.48%, Cl, 9.16%. found C, 68.03%; H, 3.89%; N, 14.22%, Cl, 9.42%.

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