Water → HCID 86664975, compound

HRID 83945

Reaction equation

HRID 83945 reaction equation
O.S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30].[CH2:33]([N:36]([CH2:40][CH:41]=[CH2:42])[CH2:37][CH:38]=[CH2:39])[CH:34]=[CH2:35].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>>[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[CH2:33]([N:36]([CH2:40][CH:41]=[CH2:42])[CH2:37][CH:38]=[CH2:39])[CH:34]=[CH2:35].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30]

Participants

8

Reactant 7

HCID 962Water2×HCID 6581Acrylic AcidHCID 7617TriallylamineHCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 99939gamma-Methyl-alpha-methylene-gamma-butyrolactoneHCID 3423265Sodium Lauryl Sulfate2×

Product 1

HCID 86664975HCID 86664975, compound

Conditions

Temperature
75 °C

Procedure

To a 150 mL round bottom flask equipped with a magnetic stir bar is added 10.00 g (0.555 mol) water and 0.115 g (3.99×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture is pre-heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 4.725 g (4.18×10−2 mol) α-methylene-γ-valerolactone, 0.250 g (4.16×10−3 mol) acrylic acid, and 0.036 g (2.62×10−4 mol) triallyl amine is added dropwise over 120 minutes. After 5 minutes of monomer mixture addition, an aqueous mixture consisting of 18.937 g (1.05 mol) water, 0.300 g (1.04×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.037 g of a 20% aqueous sodium hydroxide solution is also added dropwise over 120 minutes. After addition of both the monomer and aqueous mixtures are complete, the emulsion stirs for an additional 60 minutes, after which the reaction is cooled to room temperature and the polymer can be dried under vacuum for isolation.

Workup

  1. customTo a 150 mL round bottom flask equipped with a magnetic stir bar
  2. additionis added dropwise over 120 minutes
  3. additionAfter 5 minutes of monomer mixture addition
  4. additionis also added dropwise over 120 minutes
  5. additionAfter addition of both the monomer and aqueous mixtures
  6. temperatureafter which the reaction is cooled to room temperature
  7. customthe polymer can be dried under vacuum for isolation

Sources & evidence

ORD record
ord-277d38abaa574fc19bb845ebc2632ccd
Source dataset
uspto-grants-2014_09
Patent number
US08846817B2

Linked notes

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