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

HRID 77390

반응식

HRID 77390 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 184406222-Chloro-5-nitroisonicotinic acid수율 110.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4e907e611bb341da8e2279b2c1516cc7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841289B2

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