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Methane → HCID 21396807, Verbindung

HRID 1439326
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1439326
[NH2:1][C:2]([O:9][CH2:10][CH2:11][CH3:12])=[C:3]([C:7]#[N:8])[C:4](=[S:6])[NH2:5].OO.C>C(O)C>[NH2:5][C:4]1[S:6][N:1]=[C:2]([O:9][CH2:10][CH2:11][CH3:12])[C:3]=1[C:7]#[N:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 297MethaneHCID 784Hydrogen PeroxideHCID 85906196HCID 85906196, Verbindung

Produkt 1

HCID 21396807HCID 21396807, VerbindungAusbeute 95,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 111 g of 3-amino-2-cyano-3-propoxypropene-thioamide in 250 ml of ethanol was heated to reflux. To this stirred mixture was added 20.4 g of 30% hydrogen peroxide, at such a rate as to maintain a uniform rate of reflux. After complete addition, the reaction mixture was heated under reflux for 20 minutes. A quantity of activated charcoal was added to the reaction mixture. The reaction mixture was filtered hot and allowed to cool. The filtrate was poured into 1500 ml of water, and the solid precipitate was collected by filtration. The dried solid was recrystallized from toluene, to give 104.5 g of 5-amino-4-cyano-3-propoxyisothiazole, m.p. 122°-125°.

Aufarbeitung

  1. temperaturewas heated to reflux
  2. temperatureat such a rate as to maintain a uniform rate
  3. temperatureof reflux
  4. additionAfter complete addition
  5. temperaturethe reaction mixture was heated
  6. temperatureunder reflux for 20 minutes
  7. filtrationThe reaction mixture was filtered hot
  8. temperatureto cool
  9. additionThe filtrate was poured into 1500 ml of water
  10. filtrationthe solid precipitate was collected by filtration
  11. customThe dried solid was recrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-45ae10aa13c442d1978445655465de9c
Quelldatensatz
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04059433

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