反応式
O[C:2]1([OH:20])[C:10](=[O:11])[C:9]2[C:4](=[C:5]([N+:16]([O-:18])=[O:17])[CH:6]=[CH:7][C:8]=2[NH:12][C:13](=[O:15])[CH3:14])[C:3]1=[O:19].[Se]=O.FC(F)(F)C(O)=O.[CH:30]([C:33]1[CH:38]=[CH:37][CH:36]=[C:35]([O:39][CH3:40])[CH:34]=1)([CH3:32])[CH3:31]>O1CCOCC1.CC(O)=O>[OH:20][C:2]1([C:36]2[CH:37]=[CH:38][C:33]([CH:30]([CH3:32])[CH3:31])=[CH:34][C:35]=2[O:39][CH3:40])[C:10](=[O:11])[C:9]2[C:4](=[C:5]([N+:16]([O-:18])=[O:17])[CH:6]=[CH:7][C:8]=2[NH:12][C:13](=[O:15])[CH3:14])[C:3]1=[O:19]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
N-(2,2-dihydroxy-7-nitro-1,3-dioxo-2,3-dihydro-1H-inden-4-yl)acetamide (1.50 g, 6.4 mmol) was completely dissolved in anhydrous dioxane (15 ml). This solution was added with selenium oxide (1.56 g, 14.0 mmol) and AcOH (1.5 ml). The reaction mixture was heated for 12 hrs under reflux. After filtration at high temperature, the filtrate was concentrated to afford 1.79 g (100%). A trifluoroacetic acid solution of the resulting product was added with isopropyl-3-methoxy benzene (962 mg, 6.4 mmol) followed by stirring for 12 hours. The resulting product was extracted with ethyl acetate, and concentrated organic layer was purified using column chromatography (ethylacetate:hexane=1:1) to afford the title compound (0.52 g, 20%).
後処理
- temperatureThe reaction mixture was heated for 12 hrs
- temperatureunder reflux
- filtrationAfter filtration at high temperature
- concentrationthe filtrate was concentrated
- customto afford 1.79 g (100%)
- extractionThe resulting product was extracted with ethyl acetate, and concentrated organic layer
- customwas purified
出典と根拠
- ORDレコード
- ord-636090814dc841c0bdc11ee7db9a4840
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09346749B2
関連ノート
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