反应详情

A mixture of N-(6-acetyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-3-(4-fluoro-phenyl)-3-(3-trifluoromethyl-benzenesulfonylamino)-propionamide (161 mg, 0.286 mmol, 1.0 eq), isobutylamine (Aldrich, 126 mg, 1.72 mmol, 6.0 eq), NaBH(OAc)3 (Aldrich, 182 mg, 0.858 mmol, 3.0 eq) and glacial HOAc (J, T. Baker, 34 mg, 0.572 mmol, 2.0 eq) in ClCH2—CH2Cl (3 mL) was stirred at RT for 5 days. The reaction was quenched with saturated NaHCO3 (60 mL). The crude was extracted with CH2Cl2 (60 mL×3). The extract phase was washed with saturated NaCl, dried over Na2SO4, filtered and concentrated. Flash column chromatography (silica gel, 0-10% MeOH—CH2Cl2) afforded the title compound as a colorless thin film. MS (ESI, pos. ion) m/z: 620 (M+1).

1. customThe reaction was quenched with saturated NaHCO3 (60 mL)
2. extractionThe crude was extracted with CH2Cl2 (60 mL×3)
3. washThe extract phase was washed with saturated NaCl
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated