反应详情

3-(Cyanomethyl)-3-[4-(7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]cyclobutane-1,1-diylbis(methylene) dimethanesulfonate (0.06 g, 0.0001 mol) was reacted with sodium tetrahydroborate (0.02 g, 0.0004 mol) in DMF (0.8 mL) (˜0.5 M) at 65° C. under nitrogen for 2 h. The reaction was quenched with water, and extracted with dichloromethane. The organic layers were washed with water, dried over MgSO4, concentrated. The residue was purified with Combiflash (silica gel, 0-60% EtOAc/Hex) to give the desired product. LCMS calculated for C23H33N6OSi(M+H)+: 437.2; Found: 437.4.

1. customThe reaction was quenched with water
2. extractionextracted with dichloromethane
3. washThe organic layers were washed with water
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe residue was purified with Combiflash (silica gel, 0-60% EtOAc/Hex)