反应详情

A solution of the compound obtained in Step 2 (21.2 g, 75.26 mmol), iron powder (21.01 g, 376.29 mmol) and calcium chloride (25.06 g, 225.78 mmol) in a mixed solvent of methanol (100 mL) and water (20 mL) was stirred at 60° C. for 3 hr. To the reaction solution was added brine at room temperature, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by NH-silica gel column chromatography (solvent gradient; 10 to 50% ethyl acetate/hexane) to give 4-amino-N-(3-chloro-4-cyanophenyl)-3-methylbutanamide (6.02 g, 23.92 mmol, 31.8%) as a brown oil.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with water and saturated brine
3. customdried
4. customthe solvent was evaporated under reduced pressure
5. customThe obtained residue was purified by NH-silica gel column chromatography (solvent gradient; 10 to 50% ethyl acetate/hexane)