反应详情

A mixture of 2-bromo-benzoic acid ethyl ester (7.9 g), quinazolin-6-ylamine (5.0 g), Pd(OAc)2 (387 mg), BINAP (714 mg), and K2CO3 (26 g) in toluene (100 mL was heated at reflux for 12 h. The mixture was diluted with EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo. The crude material was purified with flash chromatography (SiO2 50% EtOAc/hexane) to obtain 2-(quinazolin-6-ylamino)-benzoic acid ethyl ester. MS (ES+): 294.0 (M+H)+. Calc'd for C17H15N3O2: 293.32.

1. temperaturewas heated
2. temperatureat reflux for 12 h
3. extractionthe aqueous layer was extracted with EtOAc
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude material was purified with flash chromatography (SiO2 50% EtOAc/hexane)