Reaktion #65147

Reaktionsgleichung

3,3-dimethyl-1,2-cyclopropanedicarboxylic acid anhydride

methylhydrazine

→

titled compound

Ausbeute 27.4%

(±)-3,7,7-Trimethyl-3,4-diazabicyclo[4.1.0]heptane-2,5-dione

Ausbeute 27.4%

Lösungsmittel

ethyl alcohol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturunder reflux for 16 hours
3. 3
   SonstigeThe solvent was removed by distillation under reduced pressure
4. 4
   Sonstigethe residue was purified by silica gel column chromatography
5. 5
   SonstigeRecrystallization from ethyl acetate/hexane

Vorschrift

In 5 ml of ethyl alcohol were added 949 mg (6.77 mmol) of 3,3-dimethyl-1,2-cyclopropanedicarboxylic acid anhydride and 0.36 ml (6.77 mmol) of methylhydrazine, and the mixture was heated under reflux for 16 hours. The solvent was removed by distillation under reduced pressure, and the residue was purified by silica gel column chromatography. Recrystallization from ethyl acetate/hexane afforded 312 mg (27.3%) of the titled compound.

Quelle