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

HRID 258566

반응식

HRID 258566 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 23978Copper촉매HCID 8150Diglyme용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7b568c3df9f444d6a72ba2742e3cce12
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04033975

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