反応式
[CH3:1][N:2]([CH3:16])[C:3]1[CH:8]=[CH:7][C:6]([NH:9]C(=O)C)=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=1.O.[OH-].[K+]>CO>[NH2:9][C:6]1[CH:7]=[CH:8][C:3]([N:2]([CH3:16])[CH3:1])=[CH:4][C:5]=1[N+:13]([O-:15])=[O:14]参加物
5
実験手順
To a solution of N-[4-(dimethylamino)-2-nitrophenyl]acetamide obtained in step 11 above (1.0 eq) in MeOH and water was added KOH (1.5 eq) at room temperature and stirred for 5 hrs. Water was added to the reaction mixture and the organic layer was separated, dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford crude product, which, on purification by column chromatography afforded the desired N-(4-amino-3-nitrophenyl)-N,N-dimethylamine. (Yield=65%).
後処理
- customthe organic layer was separated
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated under reduced pressure
- customto afford crude product, which
- customon purification by column chromatography
出典と根拠
- ORDレコード
- ord-c540b97dd5a64963ac6b323b56dcc6c9
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440830B2
関連ノート
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