Oxalic Acid → HCID 54165010、化合物
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH:8]=[CH:9]N(C)C)[C:5]([Cl:13])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].C(O)(=O)C(O)=[O:19]>C(Cl)Cl.O>[Cl:13][C:5]1[CH:4]=[C:3]([N+:14]([O-:16])=[O:15])[C:2]([Cl:1])=[CH:7][C:6]=1[CH2:8][CH:9]=[O:19]参加物
5
実験手順
2,5-Dichloro-4-(2-dimethylaminoethenyl)-nitrobenzene (10 g, 38.3 mmol) was dissolved in methylene chloride (200 ml) and stirred with a solution of oxalic acid (14.5 g, 115 mmol) in water (80 ml) at room temperature for 18 hours. The layers were separated and the aqueous layer extracted with methylene chloride (50 ml). The combined organic layers were washed with water and brine, dried over magnesium sulfate and filtered. The solution was evaporated to yield the title compound. NMR (CDCl3) δ 9.70 (s, 1), 8.01 (s, 1), 7.49 (s, 1), 3.98 (s, 2).
後処理
- customThe layers were separated
- extractionthe aqueous layer extracted with methylene chloride (50 ml)
- washThe combined organic layers were washed with water and brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customThe solution was evaporated
出典と根拠
- ORDレコード
- ord-36fbd0bb9cda4b1eade419857dcba389
- 出典データセット
- uspto-grants-1994_10
- 特許番号
- US05359068
反応ノート
読み込み中…