반응식
[CH2:1]([O:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]3[NH:24][CH2:23][CH2:22][C:21]([C:25]([O:27][CH3:28])=[O:26])=[CH:20][C:19]=3[CH:29]=2)=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH3:4].Cl[C:31]([O:33][CH2:34][CH:35]=[CH2:36])=[O:32].O>N1C=CC=CC=1.CN(C)C1C=CN=CC=1>[CH2:34]([O:33][C:31]([N:24]1[C:18]2[CH:17]=[CH:16][C:15]([C:12]3[CH:11]=[CH:10][C:9]([O:8][CH2:7][CH2:6][O:5][CH2:1][CH2:2][CH2:3][CH3:4])=[CH:14][CH:13]=3)=[CH:29][C:19]=2[CH:20]=[C:21]([C:25]([O:27][CH3:28])=[O:26])[CH2:22][CH2:23]1)=[O:32])[CH:35]=[CH2:36]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
실험 절차
In pyridine (4.3 ml) was dissolved methyl 7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (0.43 g). To the solution was added allyl chloroformate (0.23 ml), and the mixture was stirred at room temperature for 14 hours. To the mixture was added 4-dimethylaminopyridine (40 mg), and the mixture was stirred at room temperature for 2 hours. The reaction solution was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate→3/1) to give methyl 1-(allyloxycarbonyl)-7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (0.30 g).
후처리
- stirringthe mixture was stirred at room temperature for 2 hours
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried with magnesium sulfate
- customThe solvent was removed under reduced pressure
- customthe resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate→3/1)
출처 및 근거
- ORD 기록
- ord-4d0ab89b2b0f4d19a79f50693d558a67
- 출처 데이터셋
- uspto-grants-2005_08
- 특허 번호
- US06936602B1
연결된 노트
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