Phosgene → 5-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

HRID 267699Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 267699
[C:1](Cl)(Cl)=[O:2].[CH:5]1([C:12]2[S:16][C:15]([NH2:17])=[N:14][N:13]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1>C(OCC)(=O)C>[CH:5]1([C:12]2[S:16][C:15]([N:17]=[C:1]=[O:2])=[N:14][N:13]=2)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]1

Komponenten

4

Edukt 2

HCID 6371PhosgeneHCID 214478325-Cycloheptyl-2-amino-1,3,4-thiadiazole

Produkt 1

HCID 214819185-Cycloheptyl-1,3,4-thiadiazol-2-yl isocyanate

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-cycloheptyl-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-cycloheptyl-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-a790bc0395534a61a684fcf4dfd65def
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03944409

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