반응식
[CH3:1][C:2]1([CH3:19])[C:10]2[C:5](=[CH:6][C:7]([N+:15]([O-:17])=[O:16])=[C:8]([NH:11]C(=O)C)[CH:9]=2)[NH:4][C:3]1=[O:18].Br[CH2:21][C:22]1[CH:27]=[CH:26][C:25]([F:28])=[CH:24][N:23]=1.C([O-])([O-])=O.[K+].[K+]>>[NH2:11][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][C:7]=1[N+:15]([O-:17])=[O:16])[N:4]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([F:28])=[CH:24][N:23]=1)[C:3](=[O:18])[C:2]2([CH3:1])[CH3:19]참가 물질
4
실험 절차
Analogously to general procedure (I) N-(3,3-dimethyl-6-nitro-2-oxo-2,3-dihydro-1H-indol-5-yl)-acetamide (0.3 g; 1.14 mmol) is alkylated using 2-bromomethyl-5-fluoro-pyridine (0.22 g; 0.46 mmol) and K2CO3 (0.4 g; 0.23 mmol) at 35° C. for 18 h. After aqueous work-up and purification by RP chromatography the pure material (87 mg) is de-acetylated in MeOH (6 ml) using DBU (16 μl) at reflux. After aqueous work-up 5-amino-1-(5-fluoro-pyridin-2-ylmethyl)-3,3-dimethyl-6-nitro-1,3-dihydro-indol-2-one (75.0 mg) is obtained and used without further purification.
후처리
- customat 35° C.
- customfor 18 h
- customAfter aqueous work-up and purification by RP chromatography the pure material (87 mg)
- temperatureat reflux
출처 및 근거
- ORD 기록
- ord-54b3c2e388b243c1a46ad43698b2c096
- 출처 데이터셋
- uspto-grants-2010_05
- 특허 번호
- US07714010B2
연결된 노트
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