Potassium Carbonate → 2-Cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene

HRID 65589

Reaktionsgleichung

Reaktionsgleichung von HRID 65589
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:11][CH3:12])([O:9][CH3:10])=[S:8].[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[OH:21])#[N:15]>C(#N)C>[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[O:21][P:7]([O:11][CH3:12])([O:9][CH3:10])=[S:8])#[N:15]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 17304Dimethyl phosphorochloridothionateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

Produkt 1

HCID 545276212-Cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiopheneAusbeute 68,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

7 g of potassium carbonate and 8 g of O,O-dimethyl chlorothiophosphate were added to a solution of 9.8 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 24 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with benzene yielded 11 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.5375.

Aufarbeitung

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. customthe residue was chromatographed over silica gel
  4. washElution with benzene

Quellen und Nachweise

ORD-Eintrag
ord-d5f22fac622f4f12bc67103271588dd4
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128562

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