반응식
Cl.Cl.[CH3:3][NH:4][NH:5][CH3:6].C(=O)([O-])[O-].[K+].[K+].O1CCCC1.[Br:18][C:19]1[CH:20]=[C:21]([Br:43])[C:22]2[N:27]=[C:26]([C:28]3[N:29]([C:34]4[C:39]([Cl:40])=[CH:38][CH:37]=[CH:36][N:35]=4)[CH:30]=[C:31]([Br:33])[CH:32]=3)[O:25][C:24](=[O:41])[C:23]=2[CH:42]=1>O>[Br:33][C:31]1[CH:32]=[C:28]([C:26]([NH:27][C:22]2[C:21]([Br:43])=[CH:20][C:19]([Br:18])=[CH:42][C:23]=2[C:24]([N:4]([CH3:3])[NH:5][CH3:6])=[O:41])=[O:25])[N:29]([C:34]2[C:39]([Cl:40])=[CH:38][CH:37]=[CH:36][N:35]=2)[CH:30]=1참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
To a mixture of 0.42 g of N,N′-dimethylhydrazine dihydrochloride, five drops of water, 0.87 g of potassium carbonate and 10 ml of tetrahydrofuran was added 0.59 g of 6,8-dibromo-2-[4-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrrol-2-yl]-4H-3,1-benzoxazine-4-one. The resulting mixture was stirred at room temperature for 2 hours. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 0.52 g of 4-bromo-N-[4,6-dibromo-2-(N,N′-dimethylhydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrrole-2-carboxamide of the formula:
후처리
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed successively with water
- dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-bda843301c224fc7b8683dd5bb097550
- 출처 데이터셋
- uspto-grants-2011_01
- 특허 번호
- US07867949B2
연결된 노트
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