反应详情

137 mg (diethoxyphosphoryl)-acetic acid and 225 mg benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium tetrafluoroborate are added subsequently to a solution of 200 mg 6-amino-4-[(3-chloro-4-fluoro-phenyl)amino]-7-cyclopropylmethoxy-quinazoline and 0.11 ml triethylamine in 1 ml of anhydrous N,N-dimethyl-formamide. The reaction mixture is stirred for one hour at room temperature, quenched with 10 ml of water, and extracted with ethyl acetate/methanol (10:1). The combined extracts are washed with water and brine, dried over magnesium sulfate, and concentrated in vacuo. The crude product is recrystallized from diethyl ether. Yield: 190 mg (64% of theory), Melting point: 185-187° C. Mass spectrum (ESI*): m/z=537, 539 [M+H]*

1. customquenched with 10 ml of water
2. extractionextracted with ethyl acetate/methanol (10:1)
3. washThe combined extracts are washed with water and brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product is recrystallized from diethyl ether