Water → alpha-Methylene-gamma-Butyrolactone Acrylic Acid

HRID 83940

反応式

HRID 83940 の反応式
O.S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH2:25][O:24][C:22]1=[O:23].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>>[CH2:20]=[C:21]1[CH2:26][CH2:25][O:24][C:22]1=[O:23].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29]

参加物

7

反応物 6

HCID 962Water2 回HCID 6581Acrylic AcidHCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactoneHCID 3423265Sodium Lauryl Sulfate2 回

生成物 1

HCID 86664973alpha-Methylene-gamma-Butyrolactone Acrylic Acid

反応条件

温度
74 °C

実験手順

To a 50 mL round bottom flask equipped with a magnetic stir bar was added 5.890 g (0.327 mol) water and 0.090 g (3.12×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 74° C., at which time a monomer mixture consisting of 2.850 g (2.91×10−2 mol) α-methylene-γ-butyrolactone that had been previously fractionally distilled and filtered over basic alumina and 0.150 g (2.50×10−3 mol) acrylic acid was added via syringe pump over 130 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 11.130 g (0.618 mol) water, 0.185 g (6.42×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.002 g (9.24×10−6 mol) sodium persulfate, and 0.061 g of a 20% aqueous sodium hydroxide solution was also added via syringe pump over 130 minutes. After both the monomer and aqueous mixtures were added completely, the emulsion was allowed to stir for an additional 60 minutes, after which the reaction was cooled to room temperature and dried under vacuum under vacuum at 90° C. overnight. Size exclusion chromatography yielded a weight average molecular weight of 817 kDa and a polydispersity of 1.87, relative to polystyrene standards.

後処理

  1. customTo a 50 mL round bottom flask equipped with a magnetic stir bar
  2. distillationhad been previously fractionally distilled
  3. additionwas added via syringe pump over 130 minutes
  4. additionAfter 10 minutes of monomer mixture addition
  5. additionwas also added via syringe pump over 130 minutes
  6. additionAfter both the monomer and aqueous mixtures were added completely
  7. temperatureafter which the reaction was cooled to room temperature
  8. customdried under vacuum under vacuum at 90° C. overnight
  9. customSize exclusion chromatography yielded a weight average molecular weight of 817 kDa

出典と根拠

ORDレコード
ord-210f64e144794c119f7e8c8c9ef315c2
出典データセット
uspto-grants-2014_09
特許番号
US08846817B2

関連ノート

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