Reaktion #314385

ord-0e8a008ed50f42d6a81f204625829f74

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITfollowed by 4 hours
  2. 2
    workup.STIRRINGof stirring
  3. 3
    SonstigeThe obtained particles (precursor of Example 1-3) 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
    SonstigeThe particles are then dialyzed
  9. 9
    workup.ADDITIONNext, they are dispersed in methanol (70 ml), to which 1.2 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
    Temperaturthis mixture is cooled in an ice bath
  14. 14
    workup.ADDITION3 g of sodium cyanotrihydroborate is added
  15. 15
    workup.WAITfollowed by an overnight
  16. 16
    workup.STIRRINGstirring at room temperature
  17. 17
    SonstigeThe obtained particles are dialyzed in water

Vorschrift

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 1-3) 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. Next, 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, 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) modified with phosphorylcholine groups.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07560023B2uspto-grants-2009_07