StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Potassium Iodide → HCID 515415, Verbindung

HRID 1578638
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1578638
Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7].[I-].[K+].[CH2:31]([NH:34][CH2:35][CH:36]=[CH2:37])[CH:32]=[CH2:33]>O1CCCC1>[CH2:31]([N:34]([CH2:35][CH:36]=[CH2:37])[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[S:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26][N:34]([CH2:35][CH:36]=[CH2:37])[CH2:31][CH:32]=[CH2:33])=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7])[CH:32]=[CH2:33]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 4875Potassium IodideHCID 31279DiallylamineHCID 12340289HCID 12340289, Verbindung

Produkt 1

HCID 515415HCID 515415, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 22.3 g (0.05 mole) of 2,7-bis(5-chlorovaleryl)thioxanthene, 1 g of potassium iodide, 100 ml of diallylamine and 200 ml of tetrahydrofuran is placed in a Paar bomb and heated to 120°C with stirring for 24 hours. Upon cooling, the mixture is filtered and the filtrate evaporated to dryness. The resulting residue is dissolved in dilute HCl and extracted with ether. The aqueous portion is made basic, extracted with methylene chloride, dried over magnesium sulfate and filtered. The filtrate is heated to boiling, treated with charcoal, filtered and filtrate evaporated to dryness. The residue is chromatographed on a column of alumina and eluted with methylene chloride. The resulting oil is dissolved in diethyl ether, dried over molecular sieves, filtered and the ether evaporated. This process is repeated several times to yield 2,7-bis(5-diallylaminovaleryl)thioxanthene.

Aufarbeitung

  1. temperatureUpon cooling
  2. filtrationthe mixture is filtered
  3. customthe filtrate evaporated to dryness
  4. dissolutionThe resulting residue is dissolved in dilute HCl
  5. extractionextracted with ether
  6. extractionextracted with methylene chloride
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. temperatureThe filtrate is heated to boiling
  10. additiontreated with charcoal
  11. filtrationfiltered
  12. customfiltrate evaporated to dryness
  13. customThe residue is chromatographed on a column of alumina
  14. washeluted with methylene chloride
  15. dissolutionThe resulting oil is dissolved in diethyl ether
  16. customdried over molecular sieves
  17. filtrationfiltered
  18. customthe ether evaporated

Quellen und Nachweise

ORD-Eintrag
ord-c58162d67f9143d5a9fef2f6cf765fe5
Quelldatensatz
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03937835

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion