Sodium Carbonate → HCID 21948806、化合物
反応式
[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:5]=1[CH:6]=[CH:7][C:8]([CH:14]=[CH2:15])=[N:9]2)([O-])=O.C(=O)([O-])[O-].[Na+].[Na+]>C(OCC)(=O)C.[Pd]>[CH2:14]([C:8]1[CH:7]=[CH:6][C:5]2[C:10](=[CH:11][CH:12]=[CH:13][C:4]=2[NH2:1])[N:9]=1)[CH3:15]参加物
5
実験手順
1.0 g (5.0 mmol) of 5-nitro-2-vinylquinoline is dissolved in 30 ml of ethyl acetate. After 100 mg of palladium on carbon and 50 mg of sodium carbonate are added, the reaction mixture is allowed to stir for 20 hours at room temperature under hydrogen atmosphere. It is then filtered on Celite and washed with ethyl acetate. After the solvent is removed in a vacuum and after chromatography on silica gel with hexane-ethyl acetate (0-100%), then with ethyl acetate-methanol (0-30%), 720 mg (84% of theory) of the product is obtained.
後処理
- filtrationIt is then filtered on Celite
- washwashed with ethyl acetate
- customAfter the solvent is removed in a vacuum
- customafter chromatography on silica gel with hexane-ethyl acetate (0-100%), then with ethyl acetate-methanol (0-30%), 720 mg (84% of theory) of the product is obtained
出典と根拠
- ORDレコード
- ord-b96ad7346bec450087d3a2b156035681
- 出典データセット
- uspto-grants-2005_05
- 特許番号
- US06897224B2
反応ノート
読み込み中…