Imidazole → 5H,6H,7H,8H-imidazo(1,5-c)pyrimidin-5-one

反応式

[C:1]([N:8]1[CH:12]=[CH:11]N=C1)([N:3]1[CH:7]=[CH:6][N:5]=[CH:4]1)=[O:2].Cl.Cl.CN1C=C(CCN)N=C1.N1C=CN=C1>ClCCl>[CH:6]1[N:5]=[CH:4][N:3]2[C:7]=1[CH2:11][CH2:12][NH:8][C:1]2=[O:2]

参加物

反応条件

温度: 22 °C

実験手順

Carbonyldiimidazole (970.2 g) was added to a stirred suspension of [2-(1-methyl-1H-imidazol-4-yl)ethyl]amine dihydrochloride (999.9 g) (commercial eg Sigma) and imidazole (37 g) in dichloromethane (5.3 litres) at ca 22° C. The resulting white suspension was heated at reflux until reaction was complete by nmr (4 h.). Solvent (8 litres) was distilled off at atmospheric pressure whilst adding IMS-G (8 litres). Additional IMS-G (2 litres) was added and the suspension cooled to ca. 22° C. and aged at this temperature for at 2 h. The solid was collected by filtration, washed with IMS-G (2×0.5 litres), pulled dry and dried in vacuo at ca. 60° C. to yield the title compound, 478 g.