반응 #1364286
ord-3177999676e84ded8952f83ab1929edd
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The solvent was evaporated
- 2workup.ADDITIONto the residue was added ethyl acetate
- 3기타Precipitated crude crystal
- 4여과was filtered
- 5기타which 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 (1.4 g) and methyl iodide (0.58 ml) in dimethylformamide (50 ml) 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-4-carbonyl) -4-aminobenzyl) -1-methylpiperidinium iodide (Compound 96) (1.6 g) as colorless crystals.