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Potassium Carbonate → 2-Ethoxy-4-dimethoxyphosphoryloxy-5-cyano-thiazole

HRID 329204
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 329204
[CH2:1]([O:3][C:4]1[S:5][C:6]([C:10]#[N:11])=[C:7]([OH:9])[N:8]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[P:18](Cl)([O:22][CH3:23])([O:20][CH3:21])=[O:19]>CC(C)=O>[CH2:1]([O:3][C:4]1[S:5][C:6]([C:10]#[N:11])=[C:7]([O:9][P:18]([O:22][CH3:23])([O:20][CH3:21])=[O:19])[N:8]=1)[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 101863Phosphorochloridic acid, dimethyl esterHCID 214389692-Ethoxy-4-hydroxythiazole-5-carbonitrile

Produkt 1

HCID 214389862-Ethoxy-4-dimethoxyphosphoryloxy-5-cyano-thiazoleAusbeute 57,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of 17 g of 2-ethoxy-4hydroxy-5-cyano-thiazole, 14 g of potassium carbonate, 13 g of O,O-dimethyl chlorophosphate and 150 ml of acetone was stirred for 3 hours at room temperature and the mixture was concentrated to dryness. The residue was added to an aqueous sodium chloride solution which was then extracted with ethyl ether. The ether extracts were washed with an aqueous 2% sodium hydroxide solution, dried and evaporated to dryness to obtain 14.4 g of 2-ethoxy-4-dimethoxyphosphoryloxy-5-cyano-thiazole as an oil with a refractive index n D 23 = 1.5056.

Aufarbeitung

  1. concentrationthe mixture was concentrated to dryness
  2. additionThe residue was added to an aqueous sodium chloride solution which
  3. extractionwas then extracted with ethyl ether
  4. washThe ether extracts were washed with an aqueous 2% sodium hydroxide solution
  5. customdried
  6. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-d75fb1e8e60041f89ca8905dde25c868
Quelldatensatz
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04020076

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