Acetone → 1-Ethyl-4-nitrosopiperazine

HRID 2286503Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2286503
[CH2:1](I)[CH3:2].CC(C)=O.[N:8]([N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[O:9].C(=O)([O-])[O-].[K+].[K+]>O>[CH2:14]([N:13]1[CH2:2][CH2:1][N:10]([N:8]=[O:9])[CH2:11][CH2:12]1)[CH3:15]

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 21845N-Nitrosopiperazine

Produkt 1

HCID 125546241-Ethyl-4-nitrosopiperazineAusbeute 103,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Ethyl iodide (8.13 g, 0.052 mole) was added to acetone (80 ml) containing N-nitroso piperazine (6.0 g, 0.052 mole) (prepared as described in U.S. Pat. No. 2,907,767) and anhydrous potassium carbonate (7.3 g, 0.052 mole). The mixture was heated under reflux for 24 hours, cooled, treated with water (50 ml) evaporated to 1/2 volume and extracted with ether (3×150 ml). The combined extracts were dried (K2CO3) filtered and evaporated in vacuo to yield N-ethyl-N'-nitrosopiperazine (7.71 g, 98%), as a straw coloured oil.

Aufarbeitung

  1. customprepared
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 24 hours
  4. temperaturecooled
  5. customevaporated to 1/2 volume
  6. extractionextracted with ether (3×150 ml)
  7. dry with materialThe combined extracts were dried (K2CO3)
  8. filtrationfiltered
  9. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ca53af96c55a4b3ebfd9f2a20a29081c
Quelldatensatz
uspto-grants-1981_05
Patentnummer
US04267175

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