Reaktion #78183

Reaktionsgleichung

HCl dioxane

phosphoryl chloride

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

NaHCO3

→

1-Chloro-4-(4-pyridylmethyl)phthalazine

Lösungsmittel

acetonitrile

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred
2. 2
   Filtrationthe title compound filtered off

Vorschrift

Under exclusion of air, 29 g (122 mmol) 4-(4-pyridylmethyl)-1(2H)-phthalazinone [for preparation, see German Auslegeschrift no. 1061788 (published Jul. 23, 1959)] in 450 ml acetonitrile is mixed with 61 ml HCl/dioxane 4N and 28 ml (306 mmol) phosphoryl chloride and stirred for 27 h at 50° C. To the white suspension, 119 g NaHCO3 in 1.45 l water is then added dropwise under ice cooling, and the mixture is stirred and the title compound filtered off. Anal. calc.(C14H10N3Cl) C, 65.76%; H, 3.94%; N, 16.43%, Cl, 13.86%. found C, 65.40%; H, 4.12%; N, 16.45%, Cl, 13.66%; FAB MS (M+H)+=256

Quelle