Water → alpha-Methylene-gamma-Butyrolactone Acrylic Acid

HRID 83940

반응식

HRID 83940 반응식
O.S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH2:25][O:24][C:22]1=[O:23].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>>[CH2:20]=[C:21]1[CH2:26][CH2:25][O:24][C:22]1=[O:23].[C:27]([OH:31])(=[O:30])[CH:28]=[CH2:29]

참가 물질

7

반응물 6

HCID 962Water2회HCID 6581Acrylic AcidHCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactoneHCID 3423265Sodium Lauryl Sulfate2회

생성물 1

HCID 86664973alpha-Methylene-gamma-Butyrolactone Acrylic Acid

반응 조건

온도
74 °C

실험 절차

To a 50 mL round bottom flask equipped with a magnetic stir bar was added 5.890 g (0.327 mol) water and 0.090 g (3.12×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 74° C., at which time a monomer mixture consisting of 2.850 g (2.91×10−2 mol) α-methylene-γ-butyrolactone that had been previously fractionally distilled and filtered over basic alumina and 0.150 g (2.50×10−3 mol) acrylic acid was added via syringe pump over 130 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 11.130 g (0.618 mol) water, 0.185 g (6.42×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.002 g (9.24×10−6 mol) sodium persulfate, and 0.061 g of a 20% aqueous sodium hydroxide solution was also added via syringe pump over 130 minutes. After both the monomer and aqueous mixtures were added completely, the emulsion was allowed to stir for an additional 60 minutes, after which the reaction was cooled to room temperature and dried under vacuum under vacuum at 90° C. overnight. Size exclusion chromatography yielded a weight average molecular weight of 817 kDa and a polydispersity of 1.87, relative to polystyrene standards.

후처리

  1. customTo a 50 mL round bottom flask equipped with a magnetic stir bar
  2. distillationhad been previously fractionally distilled
  3. additionwas added via syringe pump over 130 minutes
  4. additionAfter 10 minutes of monomer mixture addition
  5. additionwas also added via syringe pump over 130 minutes
  6. additionAfter both the monomer and aqueous mixtures were added completely
  7. temperatureafter which the reaction was cooled to room temperature
  8. customdried under vacuum under vacuum at 90° C. overnight
  9. customSize exclusion chromatography yielded a weight average molecular weight of 817 kDa

출처 및 근거

ORD 기록
ord-210f64e144794c119f7e8c8c9ef315c2
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846817B2

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