反应详情

To a solution of (S)-5-isopropyl-1-(3-(4-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-1,2,4-triazol-3-yl)phenyl)pyrazolo[1,5-a]pyrimidin-5-yl)imidazolidin-2-one (0.23 g, 0.443 mmol) at 0° C. was added sodium hydride (0.0355 g, 0.887 mmol) and the reaction stirred 10 minutes. (2-Bromoethoxy)(tert-butyl)dimethylsilane (0.212 g, 0.887 mmol) was added and the reaction stirred for 2 hours while warming to ambient temperature. The reaction was poured onto water and extracted into EtOAc. The combined organic layers were washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. The crude material was chromatographed using 20% EtOAc/dichloromethane as eluent to yield (S)-1-(2-(tert-butyldimethylsilyloxy)ethyl)-4-isopropyl-3-(3-(4-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-1,2,4-triazol-3-yl)phenyl)pyrazolo[1,5-a]pyrimidin-5-yl)imidazolidin-2-one (0.18 g, 60%).

1. stirringthe reaction stirred for 2 hours
2. additionThe reaction was poured onto water
3. extractionextracted into EtOAc
4. washThe combined organic layers were washed with water, brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude material was chromatographed