Methylhydrazine → 3,4-Diazabicyclo[4.1.0]heptane-2,5-dione, 3,7,7-trimethyl-
反応式
[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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-2a6cd7bfa9714d75963585c41e32f66f
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05418232
反応ノート
読み込み中…