反应详情

Under exclusion of air, a suspension of 12.8 g (50 mMol) of 1-chloro-4-(4-pyridyl-methyl)-phthalazine (Example 67A.1 in WO 98/35958) and 25 g (166.8 mMol) of sodium-iodide in 0.3 l of acetone is mixed with 20 ml hydroiodic acid (55% Hl in water; 144 mMol) and stirred in the dark during 6 days at RT. Filtration and washing with acetone follow. The remaining solid is suspended in 1 l of water, neutralized with 100 ml of an 1 M Na2CO3 solution, stirred during 10 min, filtered and washed with water, yielding the title compound: An. calc. (C14H10N3I.0.05 H2O) C, 48.31%; H, 2.92%; N, 12.07%; I, 36.46%; H2O, 0.26%; An. meas. C, 48.60%; H, 3.10%; N, 12.08%; I, 36.28%; H2O, 0.28%; FAB-MS (M+H)+=348.

1. filtrationFiltration
2. washwashing with acetone
3. stirringstirred during 10 min
4. filtrationfiltered
5. washwashed with water