Water → alpha-Methylene-gamma-Butyrolactone Styrene-Acrylic Acid

HRID 83948

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HRID 83948 반응식
O.S([O-])([O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]C)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH2:25][O:24][C:22]1=[O:23].C=CC1C=CC=CC=1.C(O)(=[O:38])C=C.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].[CH:9]([CH:8]=[CH:7][C:6]([OH:5])=[O:38])=[CH:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

8

반응물 7

HCID 962Water2회HCID 6581Acrylic AcidHCID 7501StyreneHCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 68352alpha-Methylene butyrolactoneHCID 3423265Sodium Lauryl Sulfate2회

생성물 1

HCID 86664976alpha-Methylene-gamma-Butyrolactone Styrene-Acrylic Acid

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온도
73 °C

실험 절차

To a 100 mL round bottom flask equipped with a magnetic stir bar was added 8.825 g (0.490 mol) water and 0.117 g (4.06×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which time a monomer mixture consisting of 3.079 g (3.14×10−2 mol) α-methylene-γ-butyrolactone, 1.082 g styrene (1.04×10−2 mol) and 0.220 g (3.66×10−3 mol) acrylic acid was added via syringe pump over 130 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.694 g (0.927 mol) water, 0.269 g (9.33×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.041 g of a 20% aqueous sodium hydroxide solution was 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 monomodal peak with a weight average molecular weight of 104 kDa and a polydispersity of 1.96, relative to polystyrene standards. Differential scanning calorimetry showed a single first order transition at approximately 167° C.

후처리

  1. customTo a 100 mL round bottom flask equipped with a magnetic stir bar
  2. additionwas added via syringe pump over 130 minutes
  3. additionAfter 10 minutes of monomer mixture addition
  4. additionwas added via syringe pump over 130 minutes
  5. additionAfter both the monomer and aqueous mixtures were added completely
  6. temperatureafter which the reaction was cooled to room temperature
  7. customdried under vacuum under vacuum at 90° C. overnight
  8. customSize exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 104 kDa
  9. customat approximately 167° C.

출처 및 근거

ORD 기록
ord-6116eca65c064d96bbedf86154eb13da
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846817B2

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