Acrylic Acid → N-propan-2-ylprop-2-enamide;prop-2-enoic acid

HRID 227205

反応式

HRID 227205 の反応式
C(OS([O-])(=O)=O)CCCCCCCCCCC.[Na+].[CH:19]([NH:22][C:23](=[O:26])[CH:24]=[CH2:25])([CH3:21])[CH3:20].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29].C(C=CC(N)=O)C=CC(N)=O.S(OOS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+]>O>[CH:19]([NH:22][C:23](=[O:26])[CH:24]=[CH2:25])([CH3:21])[CH3:20].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29]

参加物

7

反応物 5

HCID 6581Acrylic AcidHCID 16637N-IsopropylacrylamideHCID 24412Potassium PersulfateHCID 3423265Sodium Lauryl SulfateHCID 53800990Methylene-bisacrylamide

生成物 1

HCID 157470N-propan-2-ylprop-2-enamide;prop-2-enoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

Sodium dodecylsulfate (20 mg), N-isopropylacrylamide (2.4 g), acrylic acid (382 mg), and methylenebisacrylamide (121 mg) are dissolved in 200 ml of water, and, after a 30 minute stirring at 70° C. in a nitrogen atmosphere, a polymerization initiator (potassium persulfate 9.2 mg) is added, followed by 4 hours of stirring. The obtained particles (precursor of Example 3) are purified in water by means of dialysis, and then lyophilized. These particles (700 mg) are then dispersed in tetrahydrofuran (30 ml)/dimethylformamide (10 ml), and a tetrahydrofuran (10 ml)/dimethylformamide (50 ml) solution of dicyclohexylcarbodiimide (800 mg), hydroxybenzotriazole (500 mg), and 2,2′-(ethylenedioxy)bis(ethylamine) (1.14 g) is added at room temperature, followed by an overnight stirring. The particles are then dialyzed and lyophilized. They are dispersed in methanol (70 ml), to which 1.2 g of the chemical compound of Synthetic example 1 is added, followed by a 6 hour stirring at room temperature; this mixture is cooled in an ice bath, and 3 g of sodium cyanotrihydroborate is added, followed by an overnight stirring at room temperature. The obtained particles are dialyzed in water to obtain the target N-isopropylacrylamide/acrylic acid copolymer particles (650 mg) containing phosphorylcholine groups.

後処理

  1. waitfollowed by 4 hours
  2. stirringof stirring
  3. customThe obtained particles (precursor of Example 3) are purified in water by means of dialysis
  4. additionThese particles (700 mg) are then dispersed in tetrahydrofuran (30 ml)/dimethylformamide (10 ml)
  5. additiona tetrahydrofuran (10 ml)/dimethylformamide (50 ml) solution of dicyclohexylcarbodiimide (800 mg), hydroxybenzotriazole (500 mg), and 2,2′-(ethylenedioxy)bis(ethylamine) (1.14 g) is added at room temperature
  6. waitfollowed by an overnight
  7. stirringstirring
  8. customThe particles are then dialyzed
  9. additionThey are dispersed in methanol (70 ml), to which 1.2 g of the chemical compound of Synthetic example 1
  10. additionis added
  11. waitfollowed by a 6 hour
  12. stirringstirring at room temperature
  13. temperaturethis mixture is cooled in an ice bath
  14. addition3 g of sodium cyanotrihydroborate is added
  15. waitfollowed by an overnight
  16. stirringstirring at room temperature
  17. customThe obtained particles are dialyzed in water

出典と根拠

ORDレコード
ord-c4b5cd0e365649caba71cfcaf7dc5d51
出典データセット
uspto-grants-2009_07
特許番号
US07560023B2

関連ノート

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