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Hydrochloric Acid → 4-Cyclohexyl-1,2,4-triazolidine-3,5-dione

HRID 2296386
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2296386
[C:1]([NH:4][NH:5][C:6]([NH2:8])=[O:7])(N)=[O:2].[CH:9]1(N)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.Cl>CN1CCCC1=O>[CH:9]1([N:8]2[C:6](=[O:7])[NH:5][NH:4][C:1]2=[O:2])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7965CyclohexylamineHCID 80391,2-Hydrazinedicarboxamide

Produkt 1

HCID 112638834-Cyclohexyl-1,2,4-triazolidine-3,5-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Versuchsvorschrift

118 g of hydrazodicarbonamide and 100 g of cyclohexyl amine are stirred in 100 ml of N-methyl pyrrolidone for 2 hours at 160° C., for 7 hours at 175° C. and for 10 hours at 200° C. The solvent is then distilled off in vacuo and the residue is triturated with 100 ml of a 10% sodium hydroxide solution. The deposit is isolated by filtration under suction and the filtrate is neutralised with 10% hydrochloric acid. A deposit is precipitated and is isolated by filtration under suction, washed with water and dried in vacuo, giving 132 g (76% of the theoretical yield) of 4-cyclohexyl-1,2,4-triazolidine-3,5-dione (identical with the compounds produced in accordance with Example 2).

Aufarbeitung

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is triturated with 100 ml of a 10% sodium hydroxide solution
  3. customThe deposit is isolated by filtration under suction
  4. customA deposit is precipitated
  5. customis isolated by filtration under suction
  6. washwashed with water
  7. customdried in vacuo
  8. customgiving 132 g (76% of the

Quellen und Nachweise

ORD-Eintrag
ord-56b3b84d9131429fa6176953d2e8a705
Quelldatensatz
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04429135

Notizen zur Reaktion

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