反应详情

To a mixture of 2-(4-(1H-indazol-5-ylamino)-2-[(3-phenyl)phenyl)-7-methoxyquinazolin-6-yloxy)acetic acid (0.25 g, 0.48 mmole) in DMF (1 mL)/CH2Cl2 (7 mL) was added PyBOP® (0.25 g, 0.48 mmole), and DIEA (0.186 g, 0.251 mL, 1.44 mmole). The mixture was then stirred for 15 minutes and 1-methylpiperazine (0.048 g, 0.053 mL, 0.48 mmole) was added and the reaction was stirred at RT for 3 h. The volatiles were then removed in vacuo. Upon adding CH2Cl2, the crude product precipitated and was subsequently filtered. The cake was washed with ether, hexane, CH3OH, CH2Cl2 and finally hexane. The crude product was purified by reverse phase HPLC (25 to 55% CH3CN/H2O, 90 minute run time) to yield 2-(4-(1H-indazol-5-ylamino)-2-[(3-phenyl)phenyl)-7-methoxyquinazolin-6-yloxy)-1-(4-methylpiperazin-1-yl)ethanone (0.015 g, 5%). MS 600 (M+1). HPLC retention time 5.22 mins.

1. stirringthe reaction was stirred at RT for 3 h
2. customThe volatiles were then removed in vacuo
3. additionUpon adding CH2Cl2
4. customthe crude product precipitated
5. filtrationwas subsequently filtered
6. washThe cake was washed with ether, hexane, CH3OH, CH2Cl2 and finally hexane
7. customThe crude product was purified by reverse phase HPLC (25 to 55% CH3CN/H2O, 90 minute run time)