反应详情

N-(6-{7-Methoxy-6-[3-(4-methylpiperazin-1-yl)propoxy]quinazolin-4yl-amino}benzothiazol-2-yl)benzamide was prepared by heating a mixture of N-(6-amino-benzothiazol-2-yl)benzamide (Intermediate 2, 40 mg. 0.148 μmol), 4-chloro-7-methoxy-6-[3-(4methylpiperazin-1-yl)propoxy]quinazoline (IM 8, 52 mg, 0.148 mmol), and HCl (112 μL, 4 M solution in dioxane, 0.444 mmol) in n-butanol (6 mL) to 110° C. for 5 h. Saturated sodium hydrogencarbonate solution was added and the product was extracted with ethyl acetate. After washing with water and drying over Na2SO4, the solvent was removed. The residue was taken up in little methanol, then water was slowly added. After stirring the mixture overnight, a grey solid was obtained (39 mg, 66 μmol, 45%). LC(ESI-MS: m/z=584 [M+H]+; m/z=582 [M−H]−; Rt=2.26 min.

1. temperatureby heating
2. extractionthe product was extracted with ethyl acetate
3. washAfter washing with water
4. dry with materialdrying over Na2SO4
5. customthe solvent was removed
6. additionwater was slowly added
7. customa grey solid was obtained (39 mg, 66 μmol, 45%)