반응 #653110

반응 방정식

7-(4-methylphenyl)-N-(4-(piperidinomethyl)-phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide

methyl iodide

→

1-(N-(7-(4-methylphenyl)-2,3-dihydro-1-benzoxepin-4carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   workup.ADDITIONto the residue was added ethyl acetate
3. 3
   기타Precipitated crude crystal
4. 4
   여과was filtered
5. 5
   기타which were recrystallized from ethanol-ethyl acetate

실험 절차

A solution of 7-(4-methylphenyl)-N-(4-(piperidinomethyl)-phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (1.4g) and methyl iodide (0.58ml) in dimethylformamide (50ml) was stirred at room temperature over night. The solvent was evaporated, and to the residue was added ethyl acetate. Precipitated crude crystal was filtered, which were recrystallized from ethanol-ethyl acetate to give 1-(N-(7-(4-methylphenyl)-2,3-dihydro-1-benzoxepin-4carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide (Compound 96) (1.6g) as colorless crystals.

출처