反应详情

A solution in CH2Cl2 (20 ml) of 5,7-difluoro-3-piperazin-1-yl-benzo[d]isoxazole hydrochloride (1.35 g, 4.9 mmol) and trans-[4-(2-oxo-ethyl)-cyclohexyl]-carbamic acid tert-butyl ester (1.77 g, 7.3 mmol; prepared according to WO2007/093540) was stirred 15 min at r.t. before addition of Na(AcO)3BH (1.87 g, 8.8 mmol). The reaction mixture was stirred 2 h at r.t., then sat. aq. NaHCO3 was added and the product was extracted with 3 portions of CH2Cl2. After drying (Na2SO4) and evaporation of the solvent the product was purified by flash chromatography (50 g SiO2, EtOAc/MeOH 100:0→90:10) to obtain 2.59 g (quant.) of title compound as a white solid. m/z=465.3 ([M+H]+); 409.3 ([M+H—C4H8]+).

1. extractionthe product was extracted with 3 portions of CH2Cl2
2. customAfter drying
3. custom(Na2SO4) and evaporation of the solvent the product
4. customwas purified by flash chromatography (50 g SiO2, EtOAc/MeOH 100:0→90:10)