Reaktion #171137

ord-2b76164369444b459b995558f0507ec8

Reaktionsgleichung

CCCCCCCC/C=C\CCCCCCCC(=O)[O-].[Na+]
sodium oleate
C=Cc1ccccn1
2-vinylpyridine
C=C1CCOC1=O
α-methylene-γ-butyrolactone
[Na+].[OH-]
NaOH
O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
sodium persulfate
CCCCCCCC/C=C\CCCCCCCC(=O)[O-].[Na+]
sodium oleate
O
water
O
water
C=C1CCOC1=O.C=Cc1ccccn1
α-methylene-γ-butyrolactone 2-vinylpyridine

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONare added over 210 minutes
  2. 2
    workup.STIRRINGto stir at 60° C. for an additional 90 minutes
  3. 3
    Temperaturbefore cooling to room temperature
  4. 4
    Sonstigedrying under vacuum for isolation

Vorschrift

To a dry 500 mL round bottom flask with a magnetic stir bar was added 1 g (3.28×10−3 mol) sodium oleate and 71.43 g (3.96 mol) water. The reaction is heated to 60° C. while stirring under nitrogen. After 10 minutes at 60° C., a monomer mixture consisting of 22.86 g (0.217 mol) 2-vinylpyridine and 21.33 g (0.217 mol α-methylene-γ-butyrolactone, as well as an aqueous mixture consisting of 1.14 g (3.74×10−3 mol) sodium oleate, 0.36 g (9.00×10−3 mol) NaOH, 0.36 g (1.51×10−3 mol) sodium persulfate, and 142.86 g (7.93 mol) water are added over 210 minutes. The polymerization is allowed to stir at 60° C. for an additional 90 minutes before cooling to room temperature and drying under vacuum for isolation.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846817B2uspto-grants-2014_09