Methyl 7-chloro-2-methyl-[1,2,4]triazolo[1,5-a]pyrimidine-5-carboxylate → HCID 178498634, Verbindung

HRID 1755882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1755882
Cl[C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=[C:4]([C:12]([O:14][CH3:15])=[O:13])[CH:3]=1.O.[SH2:17].[Na]>CO>[SH:17][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=[C:4]([C:12]([O:14][CH3:15])=[O:13])[CH:3]=1

Komponenten

4

Edukt 2

HCID 14852618Methyl 7-chloro-2-methyl-[1,2,4]triazolo[1,5-a]pyrimidine-5-carboxylateHCID 53442613Sodium hydrogen sulfide hydrate

Produkt 1

HCID 178498634HCID 178498634, VerbindungAusbeute 83,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Methyl 7-chloro-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate (0.80 g) (3.53 mmol) are suspended in 35 ml of methanol and treated with 0.78 g (10.6 mmol) of sodium hydrogen sulphide hydrate. After stirring at 60° C. for 5 hours the mixture is concentrated and the residue is dissolved in 20 ml of water. The solution is acidified to pH 3 with 3N aqueous hydrochloric acid. The separated product is filtered off under suction and washed with water and methanol. After recrystallization from methanol/dichloromethane there is obtained 0.66 g of methyl 7-mercapto-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate as yellow crystals of melting point 237° C. (dec.).

Aufarbeitung

  1. concentrationis concentrated
  2. dissolutionthe residue is dissolved in 20 ml of water
  3. filtrationThe separated product is filtered off under suction
  4. washwashed with water and methanol
  5. customAfter recrystallization from methanol/dichloromethane there

Quellen und Nachweise

ORD-Eintrag
ord-b36d5428d7ec4ddba2d7a016e7914e75
Quelldatensatz
uspto-grants-1995_08
Patentnummer
US05438052

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