Methanol → HCID 12877063, Verbindung

HRID 1154733Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154733
CO.[CH3:3][C:4]1[N:8]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=2)[N:7]=[C:6]([SH:18])[N:5]=1.[OH-].[Na+].S(OC)(O[CH3:25])(=O)=O>O>[CH3:3][C:4]1[N:8]([C:9]2[CH:10]=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[N:7]=[C:6]([S:18][CH3:25])[N:5]=1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 178433555HCID 178433555, Verbindung

Produkt 1

HCID 12877063HCID 12877063, VerbindungAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 80 parts of methanol are added 4.7 parts of 5-methyl-1-(4-nitrophenyl)-1H-1,2,4-triazole-3-thiol and 1.2 parts of sodium hydroxide and the whole is stirred till all solid enters solution. Then there are added 2.66 parts of dimethyl sulfate and stirring is continued for 1 hour at room temperature. 100 Parts of water are added. The precipitated product is filtered off, washed with water, dried, and crystallized from 2,2'-oxybispropane, yielding 3.3 parts (66%) of 5-methyl-3-(methylthio)-1-(4-nitrophenyl)-1H-1,2,4-triazole; mp. 121°-125° C.

Aufarbeitung

  1. stirringstirring
  2. filtrationThe precipitated product is filtered off
  3. washwashed with water
  4. customdried
  5. customcrystallized from 2,2'-oxybispropane

Quellen und Nachweise

ORD-Eintrag
ord-2262f884be054effb095e8cb4bff6eed
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04490530

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