反应详情

To a suspension of 308 mg (2.5 mMol) of 4-amino-2,6-dimethyl-pyrimidine and 694 mg (2.0 mMol) of 1-iodo-4-(4-pyridyl-methyl)-phthalazine in 20 ml of toluene, 415 mg (3.0 mMol) of K2CO3 and 231 mg (0.20 mMol) of tetrakis-(triphenylphosphin)-palladium are added, and the mixture is stirred during 1 h at RT and then 17 h at 110° C. The hot reaction mixture is filtrated, the remaining solid washed out with toluene and petrol ether and discarded. From the filtrate, product crystallizes after cooling. Filtration, washing with toluene/petrol ether and recrystallization from boiling dioxane yields the title compound: m.p 232-233° C.; An. calc.(C20H18N6·0.10 H2O) C, 69.79%; H, 5.33%; N, 24.42%; H2O, 0.52%; An. meas. C, 69.78%; H, 5.32%; N, 24.20%; H2O, 0.5%; FAB-MS (M+H)+=343.

1. additionare added
2. custom17 h
3. customat 110° C
4. filtrationThe hot reaction mixture is filtrated
5. washthe remaining solid washed out with toluene and petrol ether
6. customFrom the filtrate, product crystallizes
7. temperatureafter cooling
8. filtrationFiltration
9. washwashing with toluene/petrol ether and recrystallization