反应详情

To a stirred solution of 5-iodo-7H-pyrrolo[2,3-d]pyrimidine (Preparation 201, 735 mg, 3.00 mmol) in DMF (5 mL) at 0° C. was added to sodium hydride (132 mg, 3.30 mmol, 60% in oil). The mixture was stirred at room temperature for 30 minutes, cooled to −20° C. and 2-(trimethylsilyl)ethoxymethyl chloride (0.58 mL, 3.30 mmol) added. The reaction mixture was stirred at −20° C. for 3 hours then water (30 mL) was added. The mixture was extracted with EtOAc (2×50 mL) and the combined organic phases were dried over magnesium sulphate and evaporated under reduced pressure. The crude solid was purified by column chromatography on silica gel, eluting with a gradient of heptane:EtOAc 100:0 to 50:50), to afford the title compound as a white solid in 61% yield, 691 mg.

1. temperaturecooled to −20° C.
2. stirringThe reaction mixture was stirred at −20° C. for 3 hours
3. extractionThe mixture was extracted with EtOAc (2×50 mL)
4. dry with materialthe combined organic phases were dried over magnesium sulphate
5. customevaporated under reduced pressure
6. customThe crude solid was purified by column chromatography on silica gel
7. washeluting with a gradient of heptane:EtOAc 100:0 to 50:50),