2-Methyl-2-butanol → N,N-diethyl acrylamide acryloylmorpholine

HRID 931865Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 931865
[CH2:1]([N:3]([CH2:8][CH3:9])[C:4](=[O:7])[CH:5]=[CH2:6])[CH3:2].[C:10]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)(=[O:13])[CH:11]=[CH2:12].C(O)(CC)(C)C.N(C(C1NCCN=1)(C)C)=NC(C1NCCN=1)(C)C>>[CH2:1]([N:3]([CH2:8][CH3:9])[C:4](=[O:7])[CH:5]=[CH2:6])[CH3:2].[C:10]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)(=[O:13])[CH:11]=[CH2:12]

Komponenten

5

Edukt 4

HCID 64052-Methyl-2-butanolHCID 17583N,N-DiethylacrylamideHCID 887152,2'-Azobis(2-(2-imidazolin-2-yl)propane)HCID 98723Acryloylmorpholine

Produkt 1

HCID 131732926N,N-diethyl acrylamide acryloylmorpholine

Versuchsvorschrift

In a 300 mL three-necked flask, N,N-diethyl acrylamide (12.71 g, 0.100 mol), N-acryloylmorpholine (14.12 g, 0.100 mol), t-amyl alcohol (63.20 g), a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.0310 g, 0.124 mmol) were charged, and then equipped with a three-way stop-cock, a reflux condenser tube, a thermometer and a mechanical stirrer. The concentration of the monomer was 30% by weight. After degassing inside the three-necked flask using a vacuum pump and repeating replacement by argon three times, stirring was carried out at 70° C. for 1 hour, followed by temperature rise to 75° C. and further stirring for 4 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and the solvent was distilled off by an evaporator, and then washed once with each of n-hexane/methanol (=300 mL/80 mL, 130 mL/35 mL, 100 mL/20 mL and 100 mL/10 mL). The solid component was dried overnight by a vacuum drying oven at 60° C. Liquid nitrogen was charged and the solid component was crushed by a spatula, and then dried by a vacuum drying oven at 60° C. for 3 hours. The thus obtained copolymer had a molecular weight of Mn: 49 kD, Mw: 162 kD (Mw/Mn=3.3).

Aufarbeitung

  1. customequipped with a three-way
  2. customAfter degassing inside the three-necked flask
  3. customfollowed by temperature rise to 75° C.
  4. stirringfurther stirring for 4 hours
  5. customAfter completion of the polymerization
  6. customthe polymerization reaction solution
  7. distillationthe solvent was distilled off by an evaporator
  8. washwashed once with each of n-hexane/methanol (=300 mL/80 mL, 130 mL/35 mL, 100 mL/20 mL and 100 mL/10 mL)
  9. customThe solid component was dried overnight by a vacuum
  10. customdrying oven at 60° C
  11. additionLiquid nitrogen was charged
  12. customthe solid component was crushed by a spatula
  13. customdried by a vacuum
  14. customdrying oven at 60° C. for 3 hours

Quellen und Nachweise

ORD-Eintrag
ord-95e331f2b266489b89a69fdf9202fe9e
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09297930B2

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