反応式
Cl.Cl.[CH3:3][NH:4][NH:5][CH3:6].C(=O)([O-])[O-].[K+].[K+].[Br:13][C:14]1[CH:15]=[C:16]([C:26]2[O:31][C:30](=[O:32])[C:29]3[CH:33]=[C:34]([Cl:38])[CH:35]=[C:36]([CH3:37])[C:28]=3[N:27]=2)[N:17]([C:19]2[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][N:20]=2)[CH:18]=1>O.CN(C)C=O>[Br:13][C:14]1[CH:15]=[C:16]([C:26]([NH:27][C:28]2[C:36]([CH3:37])=[CH:35][C:34]([Cl:38])=[CH:33][C:29]=2[C:30]([N:4]([CH3:3])[NH:5][CH3:6])=[O:32])=[O:31])[N:17]([C:19]2[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][N:20]=2)[CH:18]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To a mixture of 0.29 g of N,N′-dimethylhydrazine dihydrochloride, 1 ml of water, 0.31 g of potassium carbonate and 10 ml of N,N-dimethylformamide was added 1.0 g of 2-[4-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrrol-2-yl]-6-chloro-8-methyl-4H-3,1-benzoxazine-4-one. The resulting mixture was stirred at room temperature for 6 hours. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate three times. The organic layers were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 0.26 g of 4-bromo-N-[4-chloro-2-(N,N′-dimethylhydrazinocarbonyl)-6-methylphenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrrole-2-carboxamide of the formula:
後処理
- extractionthe mixture was extracted with ethyl acetate three times
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0ba5eadd7aba4b8dbbd57508763f68cd
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07867949B2
関連ノート
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