反応式
[CH3:1][C:2]([CH3:8])([CH3:7])[C:3]([NH:5][NH2:6])=[O:4].[Cl:9][CH2:10][C:11](Cl)=[O:12]>C(OCC)(=O)C>[Cl:9][CH2:10][C:11]([NH:6][NH:5][C:3](=[O:4])[C:2]([CH3:8])([CH3:7])[CH3:1])=[O:12]参加物
4
実験手順
5.8 g (49.929 mmol) of 2,2-dimethylpropanehydrazide were dissolved in 600 ml of dry ethyl acetate and heated to reflux. 6.767 g (59.915 mmol) of chloroacetyl chloride, dissolved in 45 ml of dry ethyl acetate, were added dropwise to the solution. The mixture was stirred under reflux for 30 min. After cooling, the reaction mixture was concentrated on a rotary evaporator and the residue was dried under high vacuum. This gave 10.14 g of the title compound. The crude product was reacted further without further purification.
後処理
- temperatureheated to reflux
- additionwere added dropwise to the solution
- temperatureunder reflux for 30 min
- temperatureAfter cooling
- concentrationthe reaction mixture was concentrated on a rotary evaporator
- customthe residue was dried under high vacuum
- customThe crude product was reacted further without further purification
出典と根拠
- ORDレコード
- ord-5de56236fbe84fa7b3bc245c0078ba42
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987256B2
関連ノート
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