Phosgene → HCID 54090647, Verbindung

HRID 596736Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 596736
[C:1](Cl)(Cl)=[O:2].[CH:5]1([C:10]2[S:14][C:13]([NH2:15])=[N:12][N:11]=2)[CH2:9][CH2:8][CH2:7][CH2:6]1>C(OCC)(=O)C>[CH:5]1([C:10]2[S:14][C:13]([N:15]=[C:1]=[O:2])=[N:12][N:11]=2)[CH2:6][CH2:7][CH2:8][CH2:9]1

Komponenten

4

Edukt 2

HCID 6371PhosgeneHCID 20636875-cyclopentyl-1,3,4-thiadiazol-2-amine

Produkt 1

HCID 54090647HCID 54090647, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A saturated solution of phosgene in ethyl acetate (100 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. A slurry of 5-cyclopentyl-2-amino-1,3,4-thiadiazole (50 grams) in ethyl acetate (300 ml) is added to the reaction vessel and the resulting mixture is stirred for a period of about 16 hours, resulting in the formation of a precipitate. The reaction mixture is then purged with nitrogen gas to remove unreacted phosgene. The purged mixture is then filtered to recover the precipitate. The precipitate is then recrystallized to yield the desired product 5-cyclopentyl-1,3,4-thiadiazol-2-yl isocyanate dimer.

Aufarbeitung

  1. customequipped with a mechanical stirrer
  2. customresulting in the formation of a precipitate
  3. customThe reaction mixture is then purged with nitrogen gas
  4. customto remove unreacted phosgene
  5. filtrationThe purged mixture is then filtered
  6. customto recover the precipitate
  7. customThe precipitate is then recrystallized

Quellen und Nachweise

ORD-Eintrag
ord-1d197e8d1eeb49f8bca121c2ed0b63fc
Quelldatensatz
uspto-grants-1977_03
Patentnummer
US04012223

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