Water → HCID 178518775, Verbindung

HRID 268127

Reaktionsgleichung

Reaktionsgleichung von HRID 268127
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.[SH-:12].[K+].O>C(O)C>[SH:12][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 102109Potassium bisulfideHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

Produkt 1

HCID 178518775HCID 178518775, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 6-chloro-2,3-dihydro-s-triazolo[4,3-b]-pyridazin-3-one [P. Francavilla and F. Lauria, J. Het. Chem., 8, 415 (1971) ] (1.70 g., 0.01 mole) and potassium hydrosulfide (1.44 g., 0.02 mole) in ethanol (30 ml.) was heated in a sealed tube for 8 hours at 140°. After cooling, water (50 ml.) was added to the reaction mixture and a small amount of insoluble material was removed by filtration. The filtrate being concentrated under reduced pressure, the concentrate was acidified to pH 2 with dil. HCl to afford yellow precipitate of 6-mercapto-2,3-dihydro-s-triazolo[4,3-b]pyridazin-3-one which was collected by filtration, washed with water (10 ml.) and dried in vacuo on P2O5. Yield 1.43 g. (84%). M.p. > 300° C.

Aufarbeitung

  1. temperaturewas heated in a sealed tube for 8 hours at 140°
  2. temperatureAfter cooling
  3. customa small amount of insoluble material was removed by filtration
  4. concentrationThe filtrate being concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-32300869426342f1a6c09e7dde0ee8ee
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03946000

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