Sodium Hydroxide → HCID 178484362, Verbindung

HRID 1073814Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073814
[SH:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.[OH-].[Na+].[CH3:10][N:11]([CH3:16])[C:12](=[NH:15])[CH2:13]Cl>C(O)C>[CH3:10][N:11]([CH3:16])[C:12]([CH2:13][S:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1)=[NH:15]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 426331Ethanimidamide, 2-chloro-N,N-dimethyl-HCID 178418558HCID 178418558, Verbindung

Produkt 1

HCID 178484362HCID 178484362, VerbindungAusbeute 53,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

In 30 ml of ethanol was suspended 2.25 g of 2,5-dimercapto-1,3,4-thiadiazole, and 30 ml of 1N-sodium hydroxide solution was added to the suspension. The mixture was stirred at room temperature for 30 minutes. To the mixture was added 2.36 g of N,N-dimethylchloroacetamidine. The mixture was stirred at room temperature for an hour and concentrated under reduced pressure. The precipitating crystals were collected by filtration and washed with cold water and then a (1:1) mixture of methanol and ethyl ether to obtain 1.87 g of 2-(N,N-dimethylamidinomethylthio)-5-mercapto-1,3,4-thiadiazole as colorless crystals (mp 95°-97° C.).

Aufarbeitung

  1. additionwas added to the suspension
  2. stirringThe mixture was stirred at room temperature for an hour
  3. concentrationconcentrated under reduced pressure
  4. filtrationThe precipitating crystals were collected by filtration
  5. washwashed with cold water
  6. additiona (1:1) mixture of methanol and ethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-a9b698dfb69a4a9794909e1eeef5c81b
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04971963

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