تفاعل #314386

ord-aa333acfac484d0b82bfbab45aa0b5b8

معادلة التفاعل

CCCCCCCCCCCCOS(=O)(=O)[O-].[Na+]
Sodium dodecylsulfate
C=CC(=O)NC(C)C
N-isopropylacrylamide
C=CC(=O)O
acrylic acid
NC(=O)C=CCC=CC(N)=O
methylenebisacrylamide
O=S(=O)([O-])OOS(=O)(=O)[O-].[K+].[K+]
potassium persulfate
C=CC(=O)NC(C)C.C=CC(=O)O
N-isopropylacrylamide acrylic acid

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITfollowed by 4 hours
  2. 2
    workup.STIRRINGof stirring
  3. 3
    أخرىThe obtained particles (precursor of Example 2-2) are purified in water by means of dialysis
  4. 4
    workup.ADDITIONThese particles (700 mg) are then dispersed in tetrahydrofuran (30 ml)/dimethylformamide (10 ml)
  5. 5
    workup.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. 6
    workup.WAITfollowed by an overnight
  7. 7
    workup.STIRRINGstirring
  8. 8
    أخرىThe particles are then dialyzed
  9. 9
    workup.ADDITIONThey are dispersed in methanol (70 ml), to which 1 g of the chemical compound of Synthetic example 1
  10. 10
    workup.ADDITIONis added
  11. 11
    workup.WAITfollowed by a 6 hour
  12. 12
    workup.STIRRINGstirring at room temperature
  13. 13
    درجة الحرارةthis mixture is cooled in an ice bath
  14. 14
    workup.ADDITION2.8 g of sodium cyanotrihydroborate is added
  15. 15
    workup.WAITfollowed by an overnight
  16. 16
    workup.STIRRINGstirring at room temperature
  17. 17
    أخرىThe obtained particles are dialyzed in water

الإجراء التجريبي

Sodium dodecylsulfate (20 mg), N-isopropylacrylamide (2.7 g), acrylic acid (172 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 2-2) 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 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, 2.8 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 (620 mg) having phosphorylcholine groups directly on the particle surface.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07560023B2uspto-grants-2009_07