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Water → alpha-Methylene-gamma-Butyrolactone Acrylic Acid

HRID 83938
ノート
印刷プレビュー

反応式

HRID 83938 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]
参加物反応条件実験手順後処理出典と根拠反応ノート

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 86664973
alpha-Methylene-gamma-Butyrolactone Acrylic Acid

反応条件

温度
75 °C

実験手順

To a 250 mL round bottom flask equipped with a magnetic stir bar was added 44.080 g (2.45 mol) water and 0.523 g (1.81×10−3 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 20.81 g (2.12×10−1 mol) α-methylene-γ-butyrolactone that had been previously filtered over basic alumina and 1.100 g (1.83×10−2 mol) acrylic acid was added dropwise over 110 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 83.48 g (4.63 mol) water, 1.32 g (4.58×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.065 g (2.73×10−4 mol) sodium persulfate, and 0.18 g of a 20% aqueous sodium hydroxide solution was added dropwise over 110 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 at 90° C. overnight. Size exclusion chromatography yielded a weight average molecular weight of 191 kDa and a polydispersity of 1.62, relative to polystyrene standards.

後処理

  1. customTo a 250 mL round bottom flask equipped with a magnetic stir bar
  2. additionwas added dropwise over 110 minutes
  3. additionAfter 10 minutes of monomer mixture addition
  4. additionwas added dropwise over 110 minutes
  5. additionAfter both the monomer and aqueous mixtures were added completely
  6. temperatureafter which the reaction was cooled to room temperature
  7. customdried under vacuum at 90° C. overnight
  8. customSize exclusion chromatography yielded a weight average molecular weight of 191 kDa

出典と根拠

ORDレコード
ord-278e110c933c4c8497f4c9e5c8932920
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846817B2

反応ノート

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