Methylhydrazine → 3,4-Diazabicyclo[4.1.0]heptane-2,5-dione, 3,7,7-trimethyl-
반응식
[CH3:1][C:2]1([CH3:10])[CH:4]2[C:5]([O:7][C:8](=O)[CH:3]12)=[O:6].[CH3:11][NH:12][NH2:13]>C(O)C>[CH3:11][N:12]1[NH:13][C:5](=[O:6])[CH:4]2[CH:3]([C:2]2([CH3:10])[CH3:1])[C:8]1=[O:7]참가 물질
4
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.
후처리
- temperaturethe mixture was heated
- temperatureunder reflux for 16 hours
- customThe solvent was removed by distillation under reduced pressure
- customthe residue was purified by silica gel column chromatography
- customRecrystallization from ethyl acetate/hexane
출처 및 근거
- ORD 기록
- ord-2a6cd7bfa9714d75963585c41e32f66f
- 출처 데이터셋
- uspto-grants-1995_05
- 특허 번호
- US05418232
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