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Hydrogen iodide → 2-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

HRID 1073790
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1073790
Cl[C:2]1[N:3]=[C:4]2[S:11][C:10]([S:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[N:9][N:5]2[C:6](=[O:8])[CH:7]=1.[IH:19]>>[I:19][C:2]1[N:3]=[C:4]2[S:11][C:10]([S:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[N:9][N:5]2[C:6](=[O:8])[CH:7]=1
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Komponenten

3

Edukt 2

HCID 24841Hydrogen iodideHCID 156107907-chloro-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

Produkt 1

HCID 156107912-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-oneAusbeute 80 %

Versuchsvorschrift

A solution of 8.4 g of the thus obtained 7-chloro-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]-pyrimidin-5-one and 88.2 g of a 57% hydroiodic acid aqueous solution was heated to 95°~110° C. and stirred for 2 hours. After cooling, the solution was filtered. The residue was washed with water and dissolved in toluene. The toluene solution was washed with a sodium hydrogen carbonate aqueous solution, a sodium thiosulfate aqueous solution and water respectively and dried over anhydrous sodium sulfate. The solvent was distilled off and thus 9.8 g of 80% pure 7-iodo-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. Yield 72%.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe solution was filtered
  3. washThe residue was washed with water
  4. dissolutiondissolved in toluene
  5. washThe toluene solution was washed with a sodium hydrogen carbonate aqueous solution
  6. dry with materiala sodium thiosulfate aqueous solution and water respectively and dried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-61452dcbde6d4c72b8beffc7c8f175de
Quelldatensatz
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04971971

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