Lithium iodide → 2,6-Dichloro-4-cyanobenzoic acid
反応式
[Cl:1][C:2]1[CH:11]=[C:10]([C:12]#[N:13])[CH:9]=[C:8]([Cl:14])[C:3]=1[C:4]([O:6]C)=[O:5].[Li+].[I-]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:11]=[C:10]([C:12]#[N:13])[CH:9]=[C:8]([Cl:14])[C:3]=1[C:4]([OH:6])=[O:5]参加物
4
実験手順
To a solution of methyl 2,6-dichloro-4-cyanobenzoate (160 g, 694 mmol) in pyridine (1.5 L) at room temperature was added LiI (186 g, 1.39 mol). The mixture was heated under reflux for 2 hours, cooled to room temperature and concentrated under reduced pressure. The residue was treated with 2 N HCl (1 L) and the resulting precipitate was collected by filtration. The solid was recrystallized from DMF and water to give 2,6-dichloro-4-cyanobenzoic acid (110 g, yield: 73%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 8.18 (s, 2H). LCMS (ESI) m/z: 216.0 [M+H+].
後処理
- temperatureThe mixture was heated
- temperatureunder reflux for 2 hours
- concentrationconcentrated under reduced pressure
- additionThe residue was treated with 2 N HCl (1 L)
- filtrationthe resulting precipitate was collected by filtration
- customThe solid was recrystallized from DMF and water
出典と根拠
- ORDレコード
- ord-4f2ecd09651e4eaaa37edec68de86fe4
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08486950B2
反応ノート
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