Hydrogen Peroxide → HCID 178494688, Verbindung

HRID 1378401

Reaktionsgleichung

Reaktionsgleichung von HRID 1378401
OO.[OH:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([CH2:12][O:13][CH3:14])[N:7]=[C:6](S)[N:5]=1.S(OS([O-])=O)([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+]>>[OH:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([CH2:12][O:13][CH3:14])[N:7]=[CH:6][N:5]=1

Komponenten

5

Versuchsvorschrift

To 750 ml of 12% strength hydrogen peroxide, heated to 80° C., there were added in portions 101 g (0.5 mol) of 4-hydroxy-2-mercapto-5-methoxy-6-methoxymethylpyrimidine in such a way that a temperature of 80° C. was maintained. Stirring was then continued for 2 hours at 80° C. After cooling, solid sodium disulfite was added until potassium iodide/starch paper no longer showed a reaction with peroxide, and the mixture was then neutralized by adding potassium carbonate. The water was distilled off, and the solid residue, to which a little ethanol had been added, was then suspended in methylene chloride and subjected to filtration with suction. After concentration of the filtrate, 63 g (70% of theory) of product of melting point 141°-143° C. were obtained.

Aufarbeitung

  1. temperaturewas maintained
  2. temperatureAfter cooling
  3. distillationThe water was distilled off
  4. additionthe solid residue, to which a little ethanol had been added
  5. filtrationsubjected to filtration with suction
  6. customAfter concentration of the filtrate, 63 g (70% of theory) of product of melting point 141°-143° C. were obtained

Quellen und Nachweise

ORD-Eintrag
ord-6412ba8167d748be8a527b4d4ed93a35
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05668140

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