Sodium dichromate dihydrate → 2-Chloro-5-nitroisonicotinic acid

HRID 77390

反応式

HRID 77390 の反応式
[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

反応物 2

HCID 108005Sodium dichromate dihydrateHCID 3453642-Chloro-4-methyl-5-nitropyridine

生成物 1

HCID 184406222-Chloro-5-nitroisonicotinic acid収率 110.3%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

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

  1. additionwas added dropwise
  2. customreaction temperature
  3. customdoes not exceed 15° C
  4. additionAfter complete addition, reaction
  5. customQuenched with ice
  6. extractionextracted into ethylacetate
  7. 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

関連ノート

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