Реакция #696706

ord-39229b38af1d449abe694f37fec05bee

Реагенты

Нет

Растворители

Условия реакции

Температура
50°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISSOLUTIONAfter the acid dissolved
  2. 2
    ДругоеThe solvent and unreacted thionylchloride were removed at a reduced pressure
  3. 3
    Другоеfurther the solvent was completely removed at a high vacuum pressure

Методика

Fluorocinnamic acid (10 g, 0.06 mole) was dissolved in dichloromethane, and 8.59 g (0.07 mole) of thionylchloride was added dropwise to the solution. After the acid dissolved and the solution appeared clear, the reaction mixture was maintained at about 50° C. for 1 hour. The solvent and unreacted thionylchloride were removed at a reduced pressure and further the solvent was completely removed at a high vacuum pressure to give fluorocinnamoyl chloride. The fluorocinnamoyl chloride was dissolved in dried dichloromethane. A mixture of polyhydroxystyrene having a molecular weight of 22,000 and 6.07 g (0.06 mole) of triethylamine was dissolved in dichloromethane and a small amount of tetrahydrofuran. To this solution, the fluorocinnamoyl chloride solution was added dropwise while the temperature was maintained at 0° C. After keeping for 1 day, the resulting solution was washed with water to remove the solvent and amine salt. Polyhydroxystyrenylfluorocinnamate was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05998101uspto-grants-1999_12