反应详情

To a stirred solution of 5-chloro-3-(5-fluoro-4-(methylthio)pyrimidin-2-yl)-1-trityl-1H-pyrazolo[3,4-b]pyridine, 50, (0.078 g, 0.150 mmol) in CH2Cl2 at 0° C. was added mCPBA (0.036 g, 0.160 mmol). The mixture was kept at 0° C. for 2 hr. Then, the mixture was diluted with CH2Cl2, washed with K2CO3 (2×), dried over Na2SO4, filtered and concentrated in vacuo to provide 78 mg of the desired crude which was carried forward without further purification: LC/MS Gradient 10-90%, 0.1% formic 5 min, C18/ACN, RT=1.62 min (M+H) 554.47.

1. washwashed with K2CO3 (2×)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto provide 78 mg of the desired crude which
6. customwas carried forward without further purification
7. customLC/MS Gradient 10-90%, 0.1% formic 5 min