反応式
C[N:2](C)C=O.[Cl:6][C:7]1[C:12]2[CH:13]=[C:14]([CH2:16][CH3:17])[O:15][C:11]=2[C:10]([N:18]2[C:23](=[O:24])[CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[NH:20][C:19]2=[O:29])=[C:9]([F:30])[CH:8]=1.[N+](C1C=C([N+]([O-])=O)C=CC=1ON)([O-])=O.C(=O)([O-])[O-].[K+].[K+]>O>[Cl:6][C:7]1[C:12]2[CH:13]=[C:14]([CH2:16][CH3:17])[O:15][C:11]=2[C:10]([N:18]2[C:23](=[O:24])[CH:22]=[C:21]([C:25]([F:28])([F:26])[F:27])[N:20]([NH2:2])[C:19]2=[O:29])=[C:9]([F:30])[CH:8]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 65 °C
実験手順
80 ml of N,N-dimethylformamide was added to 3.4 g (9.0 mmol) of 3-(4-chloro-2-ethyl-6-fluorobenzofuran-7-yl)-6-trifluoromethyluracil, 2.7 g (14 mmol) of 2,4-dinitrophenoxyamine and 5.0 g (36 mmol) of potassium carbonate, followed by stirring at 60 to 70° C. for 1 hour. After completion of the reaction, the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed sequentially with water and a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 2.0 g (yield: 58%) of the desired product as white crystals. Melting point: 145-147° C.
後処理
- customAfter completion of the reaction
- extractionextracted with ethyl acetate
- washThe organic layer was washed sequentially with water
- dry with materiala saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customThen, the obtained residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-6b136cb4a742421583c4eabc5cf768e4
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06130187
関連ノート
読み込み中…