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

HRID 65588

Reaktionsgleichung

Reaktionsgleichung von HRID 65588
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8].[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[OH:23])#[N:17]>C(#N)C>[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[O:23][P:7]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8])#[N:17]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

Produkt 1

HCID 544164262-Cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiopheneAusbeute 80,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

7 g of potassium carbonate and 9.4 g of O,O-diethyl 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 filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with benzene yielded 14 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.525.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-154dc8038b1344f887f05796c8bc9dc9
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128562

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