반응식
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].[C:11](OC(=O)C)(=[O:13])[CH3:12].O.C(OCC)(=O)C>N1C=CC=CC=1>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:11](=[O:13])[CH3:12]참가 물질
6
실험 절차
To a solution of 3-bromobenzylamine hydrochloride (5.20 g) in pyridine (30 ml) was added acetic anhydride (3.2 ml) at 0° C. and the mixture was stirred at room temperature for 24 h. Water and ethyl acetate were added to the reaction mixture for partitioning, and the organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to give the title compound (4.00 g) as colorless needle crystals.
후처리
- customfor partitioning
- washthe organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine
- dry with materialdried (magnesium sulfate)
- concentrationconcentrated under reduced pressure
- customThe residue was recrystallized from hexane-ethyl acetate
출처 및 근거
- ORD 기록
- ord-35cf1564147845648b941737314ce4d1
- 출처 데이터셋
- uspto-grants-2003_02
- 특허 번호
- US06518257B1
연결된 노트
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