Water → alpha-Methylene-gamma-Butyrolactone N,N-Dimethyl Acrylamide

HRID 83950

反応式

HRID 83950 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].[CH3:27][N:28]([CH3:33])[C:29](=[O:32])[CH:30]=[CH2:31].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].[CH3:27][N:28]([CH3:33])[C:29](=[O:32])[CH:30]=[CH2:31]

参加物

7

反応物 6

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 17587N,N-DimethylacrylamideHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactoneHCID 3423265Sodium Lauryl Sulfate2 回

生成物 1

HCID 86664977alpha-Methylene-gamma-Butyrolactone N,N-Dimethyl Acrylamide

反応条件

温度
73 °C

実験手順

To a 100 mL round bottom flask equipped with a magnetic stir bar was added 8.844 g (0.491 mol) water and 0.121 g (4.20×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which time a monomer mixture consisting of 2.053 g (2.09×10−2 mol) α-methylene-γ-butyrolactone and 2.113 g (2.13×10−2 mol) N,N-dimethyl acrylamide was added via syringe pump over 120 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.658 g (0.925 mol) water, 0.264 g (9.15×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.029 g (1.22×10−4 mol) sodium persulfate, and 0.028 g of a 20% aqueous sodium hydroxide solution was added via syringe pump over 120 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 monomodal peak with a weight average molecular weight of 200 kDa and a polydispersity of 3.32, relative to polystyrene standards. Differential scanning calorimetry showed a first order transition at approximately 162° C.

後処理

  1. customTo a 100 mL round bottom flask equipped with a magnetic stir bar
  2. additionwas added via syringe pump over 120 minutes
  3. additionAfter 10 minutes of monomer mixture addition
  4. additionwas added via syringe pump over 120 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 under vacuum at 90° C. overnight
  8. customSize exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 200 kDa
  9. customat approximately 162° C.

出典と根拠

ORDレコード
ord-96cd259451dc4b65bb5a2afe28308cbf
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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