Potassium Carbonate → HCID 88832108, Verbindung

HRID 1288534Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1288534
[S:1]1[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[NH:3][C:2]1=[O:11].C(=O)([O-])[O-].[K+].[K+].[P:18](Cl)([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[S:19]>CC(C)=O>[CH2:21]([O:20][P:18]([O:11][C:2]1[S:1][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[N:3]=1)([O:23][CH2:24][CH3:25])=[S:19])[CH3:22]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 432867223,4,5,6,7,8-Hexahydro-2H-cycloheptathiazol-2-one

Produkt 1

HCID 88832108HCID 88832108, VerbindungAusbeute 37,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of 8.5 g of 2,3,5,6,7,8-hexahydro-4H-cycloheptathiazoline-2-one, 7 g of potassium carbonate and 200 ml of acetone was refluxed for 1 hour and after addition of 9.5 g of O,O-diethyl chlorothiophosphate thereto, the mixture was refluxed 24 hours. The mixture was filtered to remove mineral salts and the filtrate was distilled to dryness under reduced pressure. The residue was chromatographed over silica gel and elution with an 8-2 cyclohexane-ethyl acetate mixture gave 6 g of 2-(diethoxythiophosphoryloxy)-5,6,7,8-tetrahydro-4H-cycloheptathiazole with a refractive index of nD19 = 1.5246.

Aufarbeitung

  1. temperaturewas refluxed for 1 hour
  2. temperaturethe mixture was refluxed 24 hours
  3. filtrationThe mixture was filtered
  4. customto remove mineral salts
  5. distillationthe filtrate was distilled to dryness under reduced pressure
  6. customThe residue was chromatographed over silica gel and elution with an 8-2 cyclohexane-ethyl acetate mixture

Quellen und Nachweise

ORD-Eintrag
ord-fd872235d4ed41acb3386fff2de90dfb
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03988444

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