Hydrochloric Acid → 2-Amino-5-chloropyridin-3-ol

HRID 258566

Reaktionsgleichung

Reaktionsgleichung von HRID 258566
[NH2:1][C:2]1[C:7](Cl)=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[OH-:10].[K+].Cl.[Cl-].[Na+]>[Cu].COCCOCCOC>[NH2:1][C:2]1[C:7]([OH:10])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 14797Potassium HydroxideHCID 778863,5-Dichloro-3-pyridylamine

Produkt 1

HCID 103132002-Amino-5-chloropyridin-3-olAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23978CopperKatalysatorHCID 8150DiglymeLösungsmittel

Versuchsvorschrift

A mixture of 20 parts of 2-amino-3,5-dichloropyridine, 160 parts of glycol, 80 parts of potassium hydroxide, 1 part of copper powder and 3 parts of diethylene glycol dimethyl ether is stirred under nitrogen for 5 hours at 150°-160° C. The cooled solution is neutralised with conc. hydrochloric acid, saturated with sodium chloride and extracted twice in the warm state with ethyl acetate. The combined extracts are filtered through Hyflo, dried over magnesium sulphate and purified with active charcoal. The solvent is evaporated off to leave 12.3 parts (70% of theory) of 2-amino-3-hydroxy-5-chloropyridine, m.p. 198°-201° C.

Aufarbeitung

  1. extractionextracted twice in the warm state with ethyl acetate
  2. filtrationThe combined extracts are filtered through Hyflo
  3. dry with materialdried over magnesium sulphate
  4. custompurified with active charcoal
  5. customThe solvent is evaporated off

Quellen und Nachweise

ORD-Eintrag
ord-7b568c3df9f444d6a72ba2742e3cce12
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04033975

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