Acetaldehyde → tert-Butyl 2-ethylidenehydrazine-1-carboxylate
反応式
[C:1]([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])(=[O:4])[NH:2][NH2:3].[CH:10](=O)[CH3:11]>C(O)C>[C:6]([O:5][C:1]([NH:2][N:3]=[CH:10][CH3:11])=[O:4])([CH3:9])([CH3:8])[CH3:7]参加物
4
実験手順
A solution of tert-butyl carbazate (50.0 g, 0.38 mole) and acetaldehyde (17.5 g, 0.4 mole) in ethanol (250 mL) was refluxed for 72 h. The solution was concentrated in vacuo and dissolved in ethyl acetate. The solution was washed with water, dried (anhydrous sodium sulfate) and concentrated to afford N′-ethylidene-hydrazinecarboxylic acid tert-butyl ester (56 g) as a light yellow oil that solidified on standing. MS (ESI+) for C7H14N2O2 m/z 159.0 (M+H)+.
後処理
- concentrationThe solution was concentrated in vacuo
- dissolutiondissolved in ethyl acetate
- washThe solution was washed with water
- dry with materialdried (anhydrous sodium sulfate)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a135696105874c1c846421f7898549ec
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06960664B2
反応ノート
読み込み中…