Water → alpha-Methylene-gamma-Butyrolactone Hydroxyethyl Methacrylate 4-Vinyl Benzoic Acid

HRID 83956

反応式

HRID 83956 の反応式
O.[CH2:2]=[C:3]1[CH2:8][CH2:7][O:6][C:4]1=[O:5].[C:9]([O:14][CH2:15][CH2:16][OH:17])(=[O:13])[C:10]([CH3:12])=[CH2:11].[CH:18]([C:20]1[CH:28]=[CH:27][C:23]([C:24]([OH:26])=[O:25])=[CH:22][CH:21]=1)=[CH2:19].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>>[CH2:2]=[C:3]1[CH2:8][CH2:7][O:6][C:4]1=[O:5].[C:9]([O:14][CH2:15][CH2:16][OH:17])(=[O:13])[C:10]([CH3:12])=[CH2:11].[CH:18]([C:20]1[CH:28]=[CH:27][C:23]([C:24]([OH:26])=[O:25])=[CH:22][CH:21]=1)=[CH2:19]

参加物

6

反応物 5

HCID 962Water2 回HCID 133602-Hydroxyethyl MethacrylateHCID 140984-Vinylbenzoic acidHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactone

生成物 1

HCID 86664984alpha-Methylene-gamma-Butyrolactone Hydroxyethyl Methacrylate 4-Vinyl Benzoic 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 is added 50 g (2.78 mol) water and 1.67 g of the surfactant Abex EP-110 (Rhodia). The mixture is heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 14.70 g (1.50×10−1 mol) α-methylene-γ-butyrolactone, 19.55 g (1.50×10−1 mol) hydroxyethyl methacrylate, and 1.71 g (1.16×10−2 mol) 4-vinyl benzoic acid is added via syringe pump over 180 minutes at reflux. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.667 g (0.925 mol) water, 0.12 g (5.04×10−4 mol) sodium persulfate, is added via syringe pump over 180 minutes at reflux. After both the monomer and aqueous mixtures are completely added, the emulsion is allowed to stir for an additional 60 minutes, after which the reaction is allowed to cool to room temperature and dried under vacuum at elevated temperature for isolation.

後処理

  1. customTo a 250 mL round bottom flask equipped with a magnetic stir bar
  2. additionis added via syringe pump over 180 minutes
  3. temperatureat reflux
  4. additionAfter 10 minutes of monomer mixture addition
  5. additionis added via syringe pump over 180 minutes
  6. temperatureat reflux
  7. additionAfter both the monomer and aqueous mixtures are completely added
  8. temperatureto cool to room temperature
  9. customdried under vacuum at elevated temperature for isolation

出典と根拠

ORDレコード
ord-151d00a71a7b42c2bfaef303a222d645
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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