反应详情

A solution of the compound obtained in Step 1 of Example 48 (1.2 g, 5.44 mmol) and DBU (0.984 mL, 6.53 mmol) in 1-nitropropane (2.420 mL, 27.19 mmol) was stirred at 60° C. for 2 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 silica gel column chromatography (solvent gradient; 10 to 30% ethyl acetate/hexane) to give N-(3-chloro-4-cyanophenyl)-3-methyl-4-nitrohexanamide (1.420 g, 4.58 mmol, 84%) as a pale-yellow 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 silica gel column chromatography (solvent gradient; 10 to 30% ethyl acetate/hexane)