[Cl:1][C:2]1[N:6]2[C:7](O)=[N:8][C:9]([C:12]3[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=3[Cl:19])=[C:10]([Cl:11])[C:5]2=[N:4][CH:3]=1.P(Cl)(Cl)([Cl:23])=O.C(=O)(O)[O-].[Na+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(OCC)(=O)C>[Cl:1][C:2]1[N:6]2[C:7]([Cl:23])=[N:8][C:9]([C:12]3[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=3[Cl:19])=[C:10]([Cl:11])[C:5]2=[N:4][CH:3]=1200 mg (0.4 mmol) of 3,8-dichloro-7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidin-5-ol (Example 124A) are introduced into phosphoryl chloride (2 ml), 300 mg (1.3 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 12 h. The reaction mixture is slowly added, with vigorous stirring, to saturated sodium bicarbonate solution, and solid sodium bicarbonate (approx. 1.5 g) is added until a pH of 10 is reached. The mixture is stirred for 10 min, ethyl acetate (100 ml) is added and shaken, and the organic phase is separated off, washed with water and dried over magnesium sulphate and concentrated in a rotary evaporator. The residue is purified by silica gel chromatography (cyclohexane/ethyl acetate 10:1). 150 mg (94% of theory) of the product are obtained.
Wird geladen…
