Methanol → HCID 12877063, Verbindung

HRID 2286547Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2286547
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-fafcc9fffeb746fdaae399e4f4f78489
Quelldatensatz
uspto-grants-1981_05
Patentnummer
US04267179

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