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

HRID 227205

반응식

HRID 227205 반응식
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]

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c4b5cd0e365649caba71cfcaf7dc5d51
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560023B2

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