Chloroacetonitrile → 4-Cyanomethyl-piperazine-1-carboxylic Acid ethyl ester

HRID 16061

Reaktionsgleichung

Reaktionsgleichung von HRID 16061
[N:1]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH2:13][C:14]#[N:15].C([O-])([O-])=O.[K+].[K+]>CC#N>[CH2:10]([O:9][C:7]([N:1]1[CH2:6][CH2:5][N:4]([CH2:13][C:14]#[N:15])[CH2:3][CH2:2]1)=[O:8])[CH3:11]

Komponenten

5

Edukt 3

HCID 7856ChloroacetonitrileHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium Carbonate

Produkt 1

HCID 588605094-Cyanomethyl-piperazine-1-carboxylic Acid ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 3 g (19.0 mmol) of ethyl N-piperazinecarboxylate in 25 mL of CH3CN was added 1.57 g (1.32 mL 20.1 mmol) of 2-chloroacetonitrile and 15.6 g (95 mmol) K2CO3.1½H2O. The suspension was stirred at room temperature for 16 hours. The reaction was analyzed using TLC (35% Ethyl acetate/Hexanes, product r.f. 0.38 vs. sm r.f. of 0.02). The analysis indicated the reaction was complete. The golden yellow solution was evaporated to dryness. The residue was extracted with CH2Cl2/H2O, dried with MgSO4, and concentrated.

Aufarbeitung

  1. customThe golden yellow solution was evaporated to dryness
  2. extractionThe residue was extracted with CH2Cl2/H2O
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-629b3548fd6847feb79feba7a253e035
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07737127B2

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