反应详情

温度

85 °C

To a mixture of tert-butyl 5-(6-(2-chloroethoxy)-2-[(3-phenyl)phenyl)-7-methoxyquinazolin-4-ylamino)-1H-indazole-1-carboxylate (0.25 g, 0.40 mmole) in DMSO (2 mL) was added N,N-dimethyl-2-(methylamino)acetamide (0.232 g, 2.00 mmole) and the reaction was stirred at 85° C. for 4 h. The mixture was poured onto ice-water and the crude product was filtered. The product was then dissolved in a mixture of CH2Cl2 and CH3OH and the solution was concentrated in vacuo. The residue was purified via preparative TLC (SiO2, 10% CH2Cl2/CH3OH). To the product was added TFA (4 mL) and the reaction was stirred at RT for 2 h. The solution was concentrated in vacuo and the residue was triturated with ether, filtered and dried under vacuum to give 2-((2-(4-(1H-indazol-5-ylamino)-2-[(3-phenyl)phenyl)-7-methoxyquinazolin-6-yloxy)ethyl)(methyl)amino)-N,N-dimethylacetamide (0.178 g, 0.30 mmole, 74%). MS 602.6 (M+1). HPLC retention time 5.24 mins.

1. additionThe mixture was poured onto ice-water
2. filtrationthe crude product was filtered
3. dissolutionThe product was then dissolved in a mixture of CH2Cl2 and CH3OH
4. concentrationthe solution was concentrated in vacuo
5. customThe residue was purified via preparative TLC (SiO2, 10% CH2Cl2/CH3OH)
6. additionTo the product was added TFA (4 mL)
7. stirringthe reaction was stirred at RT for 2 h
8. concentrationThe solution was concentrated in vacuo
9. customthe residue was triturated with ether
10. filtrationfiltered
11. customdried under vacuum