반응 #65147

반응 방정식

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

methylhydrazine

→

titled compound

수율 27.4%

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

수율 27.4%

용매

ethyl alcohol

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux for 16 hours
3. 3
   기타The solvent was removed by distillation under reduced pressure
4. 4
   기타the residue was purified by silica gel column chromatography
5. 5
   기타Recrystallization from ethyl acetate/hexane

실험 절차

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.

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