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

HRID 1607548
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1607548
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.

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-5245f3016a354a309e4e38b11e0b3741
Quelldatensatz
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04866064

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