反应详情

温度

0 °C

Tert-butyl 9-trityl-9H-purin-6-ylcarbamate (93 mg, 0.195 mmol) and 50% dispersion in mineral oil NaH (9.4 mg, 0.195 mmol) were dissolved in DMF (0.2 ml) at 0° C. A solution of 3-(bromomethyl)-4-(3-fluorophenyl)-1H-isochromen-1-one (intermediate C4, 50 mg, 0.150 mmol) in DMF (0.6 mL) was then added. The reaction mixture was stirred at 0° C. for 5 min and at RT for 15 min. The reaction mixture was then diluted with EtOAc (20 mL) and washed with 0.2 M HClaqueous, sat NaClaqueous dried over Na2SO4 and concentrated under reduced pressure to give the crude yellow oil. The crude was reacted with TFA (1.5 ml) in DCM (2 ml) for 1 hrs. Then it was diluted with DCM and dried under reduced pressure to give an yellow oil. This was purified via reverse phase chromatography with a Biotage C18 30 g SNAP column (Phase A, water 95%, ACN 5%, formic acid 0.1%); Phase B ACN 95%, water 5%, formic acid 0.1%) to give the title compound (20 mg, 34.4%) as colourless solid.

1. washwashed with 0.2 M HClaqueous
2. dry with materialsat NaClaqueous dried over Na2SO4
3. concentrationconcentrated under reduced pressure
4. customto give the crude yellow oil
5. customdried under reduced pressure
6. customto give an yellow oil
7. customThis was purified via reverse phase chromatography with a Biotage C18 30 g SNAP column (Phase A, water 95%, ACN 5%, formic acid 0.1%)