Reacción #65147

Ecuación de reacción

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

methylhydrazine

→

titled compound

Rendimiento 27.4%

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

Rendimiento 27.4%

Disolventes

ethyl alcohol

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturathe mixture was heated
2. 2
   Temperaturaunder reflux for 16 hours
3. 3
   OtroThe solvent was removed by distillation under reduced pressure
4. 4
   Otrothe residue was purified by silica gel column chromatography
5. 5
   OtroRecrystallization from ethyl acetate/hexane

Procedimiento

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.

Fuente