Dimethylformamide → HCID 54385684, Verbindung

HRID 2231959Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231959
O=P(Cl)(Cl)Cl.[NH2:6][C:7]1[S:11][N:10]=[C:9]([C:12]([NH2:14])=O)[C:8]=1[C:15]([NH2:17])=O.[CH3:18][N:19]([CH3:22])[CH:20]=O>>[CH3:18][N:19]([CH3:22])[CH:20]=[N:6][C:7]1[S:11][N:10]=[C:9]([C:12]#[N:14])[C:8]=1[C:15]#[N:17]

Komponenten

4

Edukt 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 21285250HCID 21285250, Verbindung

Produkt 1

HCID 54385684HCID 54385684, VerbindungAusbeute 93 %

Versuchsvorschrift

10.1 parts of phosphorus oxytrichloride are added dropwise to 30 parts of dimethylformamide at 0° C., and the mixture is then stirred for a further 0.5 hour at this temperature. 3.7 parts of 5-aminoisothiazole-3,4-dicarboxamide are then introduced, a little at a time, into this solution while cooling with ice. The mixture is stirred for a further 2 hours at room temperature, after which it is poured into 100 parts of ice water. The precipitate is filtered off under suction, washed with water and dried to give 3.8 parts (93% of theory) of N,N-dimethyl-N'-(3,4-dicyanoisothiazol-5-yl)-formamidine.

Aufarbeitung

  1. temperaturea little at a time, into this solution while cooling with ice
  2. stirringThe mixture is stirred for a further 2 hours at room temperature
  3. filtrationThe precipitate is filtered off under suction
  4. washwashed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d95fc5374a504742a1142f2c6328272c
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04785116

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