반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].S(Cl)(Cl)=O.[Br:21][C:22]1[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=1[NH2:29].C(N(CC)CC)C>C(Cl)Cl.CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([C:14](=[O:16])[NH:29][C:23]2[CH:24]=[CH:25][C:26]([F:28])=[CH:27][C:22]=2[Br:21])[CH2:12][CH2:13]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]참가 물질
반응물 4
생성물 1
시약·촉매·용매 3
실험 절차
Piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (16.5 g, 72.00 mmol) was dissolved in dry methylene chloride (100 mL) and dry pyridine (15 mL). To the reaction mixture was then added thionyl chloride (10.28 g, 86.40 mmol) under nitrogen atmosphere and the reaction mixture was stirred at room temperature for 30 minutes. To the reaction mixture was then added successively, under nitrogen atmosphere, 2-bromo-4-fluoro-phenylamine (15.0 g, 79.00 mmol), dry triethylamine (25.50 g, 252.0 mmol), dry methylene chloride (120 mL), 4-(dimethylamino)pyridine (0.87 g, 7.20 mmol) and the reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was then partitioned with aqueous 2N HCl and tert-butyl methyl ether. The organic layer was washed with aqueous 2N HCl, aqueous NaHCO3, brine, dried with Na2SO4, filtered and the solvent evaporated in vacuo to yield the title compound as a solid.
후처리
- additionTo the reaction mixture was then added successively, under nitrogen atmosphere
- customThe reaction mixture was then partitioned with aqueous 2N HCl and tert-butyl methyl ether
- washThe organic layer was washed with aqueous 2N HCl, aqueous NaHCO3, brine
- dry with materialdried with Na2SO4
- filtrationfiltered
- customthe solvent evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-8e2005afd5824055b07c184c86d6bd04
- 출처 데이터셋
- uspto-grants-2010_02
- 특허 번호
- US07655670B2
연결된 노트
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