反应详情

To a flask containing intermediate 2 (0.00285 mol) was added ether. To this homogeneous solution was added HCl in diethyl ether (1M; 0.00855 mol). The solvent was evaporated and 1,4-dioxane (20 ml) was added. Finally, 4-aminobenzonitrile (0.00291 mol) and 1,4-dioxane (15 ml) were added and the reaction mixture was stirred and refluxed for seven days. The solvent was evaporated, the residue dissolved in CH2Cl2, washed with 1 M NaOH, and the solvent evaporated. The residue was dissolved in CH2Cl2 (10 ml) and the precipitate was filtered off and dried, yielding 0.15 g (13%) of 4-[[5-bromo-4-[(2,4,6-trimethylphenyl)amino]-2-pyrimidinyl]amino]benzonitrile (comp. 3).

1. customThe solvent was evaporated
2. addition1,4-dioxane (20 ml) was added
3. temperaturerefluxed for seven days
4. customThe solvent was evaporated
5. dissolutionthe residue dissolved in CH2Cl2
6. washwashed with 1 M NaOH
7. customthe solvent evaporated
8. dissolutionThe residue was dissolved in CH2Cl2 (10 ml)
9. filtrationthe precipitate was filtered off
10. customdried