Hydrochloric Acid → 2-Methylidenebutanedioic acid--prop-2-enoic acid (1/1)

HRID 249225

Reaktionsgleichung

Reaktionsgleichung von HRID 249225
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[C:6]([OH:14])(=[O:13])[C:7]([CH2:9][C:10]([OH:12])=[O:11])=[CH2:8].Cl>O>[CH2:3]=[CH:2][C:1]([OH:5])=[O:4].[CH2:8]=[C:7]([C:6]([OH:14])=[O:13])[CH2:9][C:10]([OH:12])=[O:11]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 811Itaconic acidHCID 6581Acrylic Acid

Produkt 1

HCID 1615092-Methylidenebutanedioic acid--prop-2-enoic acid (1/1)Ausbeute 296,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

Acrylic acid (20.000 g, 0.27755 mole), itaconic acid (4.0121 g, 0.038386 mole), Wako V-50 (0.0837 g, 0.308 millimole), and 150 ml of water, which has been acidified to pH 2.0 with hydrochloric acid are added to a 250 ml three-necked round-bottomed flask. The necks are fitted with a thermometer, a stopper, and a gas inlet/outlet adapter capable of bubbling gas through a liquid in the flask and venting it. The solution is deaerated by passage of nitrogen gas and is then placed under an atmosphere of argon. The solution is heated to 55° C. and is maintained at this temperature for 15 hours. The viscous solution of copolymer is cooled to ambient temperature and is dialyzed against distilled water overnight (Spectrapor 3 tubing with molecular weight cut-off at 3500) to remove any unreacted monomers. The dialyzed solution is freeze dried to give 23.00 g of poly(acrylic acid-itaconic acid) copolymer as a colorless solid. The mass average molecular weight, as determined by low angle laser light scattering in 0.2 Molar sodium chloride in water (refractive index=1.3344, dn /dc --0.1683), is 896,100.

Aufarbeitung

  1. additionare added to a 250 ml three-necked round-bottomed flask
  2. customThe necks are fitted with a thermometer
  3. customa stopper, and a gas inlet/outlet adapter capable of bubbling gas through a liquid in the flask
  4. temperatureis maintained at this temperature for 15 hours
  5. temperatureThe viscous solution of copolymer is cooled to ambient temperature
  6. customis dialyzed
  7. distillationagainst distilled water overnight (Spectrapor 3 tubing with molecular weight cut-off at 3500)
  8. customto remove any unreacted monomers
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1f30a51eadaf483e8bf82aa0e389c56b
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05213789

Verknüpfte Notizen

Wird geladen…