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0 °C

To a mixture of 1.0 M of lithium tetrahydroaluminate in THF (11.3 mL. 11.3 mmol) in THF (40 mL) was added drop-wise, a solution of 4-[1-(1-methyl-2-oxo-2-piperazin-1-ylethyl)-1H-pyrazol-4-yl]-7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidine (2.57 g, 5.64 mmol) in THF (20 mL). The mixture was refluxed for 30 min. The mixture was cooled at 0° C., quenched with 0.44 mL of water, followed by 0.44 mL of 15% NaOH, then 1.32 mL of water. The mixture was stirred at RT for 30 min, filtered through Celite. The filtrate was dried over sodium sulfate, concentrated to dryness under reduced pressure. The resultant residue was purified on silica gel, eluting with 0 to 10% methanol (containing 10% 2M NH3/EtOH) in dichloromethane, to give the desired product (690 mg, 27.7%). LCMS calculated for C22H36N7OSi (M+H)+: m/z=442.3; Found: 442.3.

1. additionwas added drop-wise
2. temperatureThe mixture was refluxed for 30 min
3. customquenched with 0.44 mL of water
4. filtrationfiltered through Celite
5. dry with materialThe filtrate was dried over sodium sulfate
6. concentrationconcentrated to dryness under reduced pressure
7. customThe resultant residue was purified on silica gel
8. washeluting with 0 to 10% methanol (containing 10% 2M NH3/EtOH) in dichloromethane