Potassium Carbonate → 5-Butoxy-2-cyanothiophen-3-yl diethyl phosphate

HRID 65590

Reaktionsgleichung

Reaktionsgleichung von HRID 65590
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[O: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])=[O:8])#[N:17]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 13139Diethyl chlorophosphateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

Produkt 1

HCID 213179365-Butoxy-2-cyanothiophen-3-yl diethyl phosphateAusbeute 93,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

7.7 g of potassium carbonate and 8.6 g of O,O-diethyl chlorophosphate were added to a solution of 11 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 16 hours at room temperature and was then filtered. The filtrate was evaporated to dryness and the residue was taken up in ethyl ether. The ether phase was washed with an aqueous solution of 100 g/l of sodium chloride and then with an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The solution was dried, treated with activated carbon, filtered and evaporated to dryness under reduced pressure to obtain 15.5 g of 2-cyano-3-(diethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.500.

Aufarbeitung

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. washThe ether phase was washed with an aqueous solution of 100 g/l of sodium chloride
  4. additionwith an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride
  5. customThe solution was dried
  6. additiontreated with activated carbon
  7. filtrationfiltered
  8. customevaporated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e7487320950f418a9e636fd700ecdb7c
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128562

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