反应详情

温度

75 °C

(S)-2-(1-((5-(1H-Pyrazol-4-yl)-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)ethyl)-5-methyl-3-phenylpyrrolo[2,1-f][1,2,4]triazin-4(3H)-one (43 mg, 0.07 mmol) and 2-chloro-N,N-dimethylethanamine chlorhydrate (43 mg, 0.30 mmol) were dissolved in DMF (3 ml) and cesium carbonate (240 mg, 0.74 mmol) was added. After stirring the mixture at 75° C. for 3.5 h, the solvent was evaporated under reduced pressure and the residue was suspended in water and extracted with dichloromethane (×3). The organic phase was successively washed with water and brine, dried over magnesium sulphate, filtered and the solvent evaporated under reduced pressure. The residue was purified using SP1® Purification System (0% to 3%, dichloromethane-methanol) to obtain 31 mg (57% yield) of the title compound as a brown solid. Purity 90%.

1. customthe solvent was evaporated under reduced pressure
2. extractionextracted with dichloromethane (×3)
3. washThe organic phase was successively washed with water and brine
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. customthe solvent evaporated under reduced pressure
7. customThe residue was purified
8. customSP1® Purification System (0% to 3%, dichloromethane-methanol)