Hydrochloric Acid → (S)-1-acetyl-2-methyl-4-nitrosopiperazine

HRID 1596209Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1596209
[C:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][C@@H:5]1[CH3:10])(=[O:3])[CH3:2].Cl.[N:12]([O-])=[O:13].[Na+].[OH-].[Na+]>O>[C:1]([N:4]1[CH2:9][CH2:8][N:7]([N:12]=[O:13])[CH2:6][C@@H:5]1[CH3:10])(=[O:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23668193Sodium NitriteHCID 54446440(2S)-N-acetyl-2-methylpiperazine

Produkt 1

HCID 45085766(S)-1-acetyl-2-methyl-4-nitrosopiperazineAusbeute 68,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a slurry of (S)-1-acetyl-2-methylpiperazine (424 mg) in water (2.5 ml) was added concentrated hydrochloric acid (0.9 ml) dropwise below 25° C. A solution of sodium nitrite (227 mg) in water (2 ml) was added dropwise at 0° C. The mixture was stirred at 0° C. for 2 hours. A solution of sodium hydroxide (409 mg) in water (6 ml) was added dropwise at 0° C. The mixture was extracted with chloroform, washed with water, dried and evaporated to give (S)-1-acetyl-2-methyl-4-nitrosopiperazine (350 mg). This product was used for next step without purification.

Aufarbeitung

  1. extractionThe mixture was extracted with chloroform
  2. washwashed with water
  3. customdried
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-2db1d6d7dcb8418f837c126d3bcfd1db
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06291464B1

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