Sodium dichromate dihydrate → 2-Chloro-5-nitroisonicotinic acid
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[OH2:12].[OH2:13].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[C:6]([C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1)[C:8]([OH:13])=[O:12]参加物
4
実験手順
2-chloro-4-methyl-5-nitropyridine (1.0 g, 5.8 mmol) was cooled using an ice water bath. Sodium dichromate dihydrate (3.45 g, 11.6 mmol) dissolved in sulphuric acid (50 mL) was added dropwise, ensuring reaction temperature does not exceed 15° C. After complete addition, reaction allowed to warm to room temperature and stirred overnight. Quenched with ice, extracted into ethylacetate and concentrated under reduced pressure to afford 2-chloro-5-nitroisonicotinic acid (1.3 g, 6.4 mmol).
後処理
- additionwas added dropwise
- customreaction temperature
- customdoes not exceed 15° C
- additionAfter complete addition, reaction
- customQuenched with ice
- extractionextracted into ethylacetate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-4e907e611bb341da8e2279b2c1516cc7
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841289B2
反応ノート
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