反応式
O.S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30].[CH2:33]([N:36]([CH2:40][CH:41]=[CH2:42])[CH2:37][CH:38]=[CH2:39])[CH:34]=[CH2:35].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>>[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[CH2:33]([N:36]([CH2:40][CH:41]=[CH2:42])[CH2:37][CH:38]=[CH2:39])[CH:34]=[CH2:35].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30]参加物
反応条件
- 温度
- 75 °C
実験手順
To a 150 mL round bottom flask equipped with a magnetic stir bar is added 10.00 g (0.555 mol) water and 0.115 g (3.99×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture is pre-heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 4.725 g (4.18×10−2 mol) α-methylene-γ-valerolactone, 0.250 g (4.16×10−3 mol) acrylic acid, and 0.036 g (2.62×10−4 mol) triallyl amine is added dropwise over 120 minutes. After 5 minutes of monomer mixture addition, an aqueous mixture consisting of 18.937 g (1.05 mol) water, 0.300 g (1.04×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.037 g of a 20% aqueous sodium hydroxide solution is also added dropwise over 120 minutes. After addition of both the monomer and aqueous mixtures are complete, the emulsion stirs for an additional 60 minutes, after which the reaction is cooled to room temperature and the polymer can be dried under vacuum for isolation.
後処理
- customTo a 150 mL round bottom flask equipped with a magnetic stir bar
- additionis added dropwise over 120 minutes
- additionAfter 5 minutes of monomer mixture addition
- additionis also added dropwise over 120 minutes
- additionAfter addition of both the monomer and aqueous mixtures
- temperatureafter which the reaction is cooled to room temperature
- customthe polymer can be dried under vacuum for isolation
出典と根拠
- ORDレコード
- ord-277d38abaa574fc19bb845ebc2632ccd
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846817B2
関連ノート
読み込み中…