反应详情

To a stirred solution of 5-pyrimidin-2-yl-1-({4-[5-(2,2,2-trifluoroethoxy)pyrimidin-2-yl]piperazin-1-yl}sulfonyl)pentan-2-one (9.47 g, 19.4 mmol) in DCM/MeOH (100 mL/100 mL) was added NaBH4 (807 mg, 21.3 mmol) portionwise and the reaction stirred at room temperature. The reaction was then quenched by addition of a saturated solution of NH4Cl (250 mL) and the organics removed in vacuo. The aqueous residue was then extracted with EtOAc (2×250 mL), combined organics washed with brine (250 mL), dried (MgSO4), filtered and concentrated in vacuo to give 5-pyrimidin-2-yl-1-({4-[5-(2,2,2-trifluoroethoxy)pyrimidin-2-yl]piperazin-1-yl}sulfonyl)pentan-2-ol as a white solid (9.10 g, 18.6 mmol, 96%).

1. customThe reaction was then quenched by addition of a saturated solution of NH4Cl (250 mL)
2. customthe organics removed in vacuo
3. extractionThe aqueous residue was then extracted with EtOAc (2×250 mL)
4. washcombined organics washed with brine (250 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo