反应详情

To an ice-cooled solution of 494 mg (0.852 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-[6-(3-oxo-morpholin-4-yl)-4-o-tolyl-pyridin-3-yl]-isobutyramide in 5 ml methanol and 5 ml tetrahydrofuran were added 635 mg (1.70 mmol) cerium(III)chloride heptahydrate. After stirring for 5 min, 64 mg (1.70 mmol) sodium borohydride were added in two portions within 2 min. After stirring for 3 h at 0° C., 1 ml acetone was added and stirring was continued for 10 min. The solvent was removed, the residue was re-dissolved in ethyl acetate and the organic phase was washed with saturated sodium carbonate solution, dried (magnesium sulfate) and evaporated. The crude material was purified by flash-chromatography to give 87 mg (16%) ofthe title compound as white crystals. MS m/e (%): 582 (M+H+, 100).

1. stirringAfter stirring for 3 h at 0° C.
2. stirringstirring
3. waitwas continued for 10 min
4. customThe solvent was removed
5. dissolutionthe residue was re-dissolved in ethyl acetate
6. washthe organic phase was washed with saturated sodium carbonate solution
7. dry with materialdried (magnesium sulfate)
8. customevaporated
9. customThe crude material was purified by flash-chromatography