反应详情

To a solution of 7-(4-dimethylaminophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (0.15g), 4-(N-methyl-N-(tetrahydropyran-4-yl)aminomethyl)aniline (0.11g) and triethylamine (0.2ml) in dimethylformamide (15ml) was added diethyl cyano-phosphate (0.11ml) under ice-cooling, and the mixture was stirred under nitrogen atmosphere at room temperature over night. The solvent was evaporated, and the residue was purified with silica gel column (methanol/ethyl acetate/triethylamine) to give crude crystals, which were recrystallized from ethyl acetate-hexane to give 7-(4-dimethylaminophenyl)-N-(4-((N-tetrahydropyran-4-yl-N-methylamino)methyl)-phenyl) 2,3-dihydro-1-benzoxepine-4-carboxamide (Compound 149) (0.07g) as pale brown crystals.

1. temperaturecooling
2. customThe solvent was evaporated
3. customthe residue was purified with silica gel column (methanol/ethyl acetate/triethylamine)
4. customto give crude crystals, which
5. customwere recrystallized from ethyl acetate-hexane