Reaktion #40761

Reaktionsgleichung

H2O2

NaClO

C-(1-Aminomethyl-cyclohexyl)-methylamine

→

2,3-Diaza-spiro[4.5]dec-2-ene

Lösungsmittel

H2O

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled in an ice bath
2. 2
   Sonstigethe ice bath was removed
3. 3
   ExtraktionExtraction with DCM
4. 4
   Trocknendrying over Na2SO4 and evaporation under reduced pressure
5. 5
   Sonstigeyielded 8.7 g of a clear, light-yellow liquid

Vorschrift

C-(1-Aminomethyl-cyclohexyl)-methylamine (10.0 g) was taken up in a mixture of H2O (40 mL) and MeOH (10 mL), and cooled in an ice bath. Simultaneously, H2O2 (44.3 mL of a 30% solution, 6 equiv.) and NaClO (125.5 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred for 45 min. at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure, yielded 8.7 g of a clear, light-yellow liquid. 1H NMR (400 MHz, CDCl3) δ 1.24-1.53 (m, 10H), 4.17 (s, 4H).

Quelle