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Diethyl Ether → HCID 178486115, Verbindung

HRID 1578997
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1578997
[Cl-].[CH3:2][N:3]([S+:5]([N:9]([CH3:11])[CH3:10])[N:6]([CH3:8])[CH3:7])[CH3:4].[O-:12][C:13]#[N:14].[Na+].CCOCC>CO>[O-:12][C:13]#[N:14].[CH3:2][N:3]([S+:5]([N:9]([CH3:11])[CH3:10])[N:6]([CH3:8])[CH3:7])[CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 517096Sodium CyanateHCID 86733077HCID 86733077, Verbindung

Produkt 1

HCID 178486115HCID 178486115, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 10 g (0.05 mole) of tris(dimethylamino)sulfonium chloride and 3.6 g (0.055 mole) powdered sodium cyanate in 100 ml methanol was stirred at room temperature (25°) for 3 days. Ether, 300 ml, was added, and the precipitated sodium chloride was filtered off. The filtrate was evaporated to dryness under reduced pressure and the residue was redissolved in acetonitrile, filtered, and then precipitated by the addition of ether. The precipitate was collected on a filter, washed with ether, and dried under dry nitrogen to give 9.27 g (90%) of tris(dimethylamino)sulfonium cyanate as a white crystalline powder, m.p. 202°-204°.

Aufarbeitung

  1. filtrationthe precipitated sodium chloride was filtered off
  2. customThe filtrate was evaporated to dryness under reduced pressure
  3. dissolutionthe residue was redissolved in acetonitrile
  4. filtrationfiltered
  5. customprecipitated by the addition of ether
  6. customThe precipitate was collected on a filter
  7. washwashed with ether
  8. customdried under dry nitrogen

Quellen und Nachweise

ORD-Eintrag
ord-7cee66f468644d9985726c8e44ebeb95
Quelldatensatz
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03940402

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