反应详情

温度

100 °C

600 mg (2.47 mmol) of 5-(4-amino-2-fluorophenoxy)-1H-indazole (from example XII) are suspended in 100 ml of water. 510 mg (2.47 mmol) of 4-chloro-6-(4-pyridinyl)-2-pyrimidineamine (from example XXIX) and 0.25 ml of concentrated aqueous hydrogen chloride solution are added, and the mixture is stirred at 100° C. overnight. For work-up, the reaction solution was made alkaline with saturated sodium bicarbonate solution and extracted 3× with ethyl acetate. The precipitate obtained contains crude product and is filtered off with suction. The organic phase is dried with sodium sulfate and concentrated using a rotary evaporator. The residue is combined with the precipitate and purified by preparative HPLC.

1. extractionextracted 3× with ethyl acetate
2. customThe precipitate obtained
3. filtrationis filtered off with suction
4. dry with materialThe organic phase is dried with sodium sulfate
5. concentrationconcentrated
6. customa rotary evaporator
7. custompurified by preparative HPLC