反应详情

A suspension of N-(4-chloromethylphenyl)-7—(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (0.1 g), amino-methylcyclohexane (0.05 g) and potassium carbonate (0.1 g) in dimethylformamide (10 ml) was stirred at room temperature over night. The solvent. was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride solution, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column (ethyl acetate/methanol/triethylamine) to give crude crystals, which were recrystallized from ethyl acetate-hexane to give N-(4—((cyclohexylmethyl)aminomethyl)phenyl)-7—(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (Compound 122) (0.06 g) as colorless crystals.

1. customwas evaporated
2. additionto the residue was added water
3. extractionThe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with water and saturated sodium chloride solution
5. dry with materialdried with anhydrous magnesium sulfate
6. customUnder reduced pressure, the solvent was evaporated
7. customthe residue was purified with silica gel column (ethyl acetate/methanol/triethylamine)
8. customto give crude crystals, which
9. customwere recrystallized from ethyl acetate-hexane