Реакция #426466

ord-d5f2995ff3554ab88448916b8364c38c

Растворители

Условия реакции

Температура
-70°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеIn a 2 L reaction vessel
  2. 2
    Другоеequipped with a stirrer
  3. 3
    Другоеpolymerization
  4. 4
    Другоеthe solution was reacted for 2.0 hours
  5. 5
    Другоеthe reaction was terminated
  6. 6
    workup.ADDITIONby adding a large amount of methanol
  7. 7
    ДругоеAfter removing the solvent
  8. 8
    workup.DISSOLUTIONthe like from the reaction solution, a polymer was dissolved in toluene
  9. 9
    Промывкаwashed twice with water
  10. 10
    workup.ADDITIONThis toluene solution was added to the methanol mixture
  11. 11
    Другоеprecipitating a polymer
  12. 12
    Сушкаthe resultant polymer was dried at 60° C. for 24 hours

Методика

In a 2 L reaction vessel equipped with a stirrer, 589 mL of methylcyclohexane (dried over molecular sieves), 613 mL of n-butyl chloride (dried over molecular sieves) and 0.550 g of cumyl chloride were charged. After cooling the reaction vessel to −70° C., 0.35 mL of a-picoline (2-methylpyridine) and 179 mL of isobutylene were added. Further, 9.4 mL of titanium tetrachloride was added to start polymerization, and then the solution was reacted for 2.0 hours while being stirred at −70° C. Next, 59 mL of styrene was added into the reaction vessel and the reaction was continued for 60 minutes, and then the reaction was terminated by adding a large amount of methanol. After removing the solvent and the like from the reaction solution, a polymer was dissolved in toluene and washed twice with water. This toluene solution was added to the methanol mixture, thereby precipitating a polymer, and the resultant polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08893756B2uspto-grants-2014_11