Hydrochloric Acid → N-[3-(dimethylamino)propyl]acrylamide acrylamide

HRID 379501

Reaktionsgleichung

Reaktionsgleichung von HRID 379501
[CH3:1][N:2]([CH3:11])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:10])[CH:8]=[CH2:9].[C:12]([NH2:16])(=[O:15])[CH:13]=[CH2:14].Cl.Cl.N(C(C(=N)N)(C)C)=NC(C(=N)N)(C)C.Cl>O.C(O)C.C(O)(C)C>[CH3:11][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:10])[CH:8]=[CH2:9].[C:12]([NH2:16])(=[O:15])[CH:13]=[CH2:14]

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 6579AcrylamideHCID 763442,2'-Azobis(2-methylpropanimidamide) dihydrochlorideHCID 77452N,N-Dimethylaminopropyl acrylamide

Produkt 1

HCID 86757471N-[3-(dimethylamino)propyl]acrylamide acrylamide

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A solution of N-[3-(dimethylamino)propyl]acrylamide (30.0 g) and acrylamide (13.6 g) in deionized water (40 mL) and ethanol (40 mL) was heated to 60° C. under a nitrogen atmosphere. When the solution reached 60° C., 2,2′-azobis(2-amidinopropane)dihydrochloride (2.2 g of a 20 percent aqueous solution) was added. Heating was continued for 18 hours under a nitrogen atmosphere. After cooling to room temperature, the reaction solution was dissolved in isopropanol (150 mL), and concentrated HCl (31.5 g) was added with stirring. The solution was decanted from the precipitated polymer. The polymer was suspended in isopropanol (500 mL), stirred for at least 15 minutes, and allowed to settle. After decanting, the polymer was similarly washed an additional 3 times with isopropanol. The washed polymer was dried in a forced-air oven at 70° C. to afford 68.2 g.

Aufarbeitung

  1. customreached 60° C.
  2. temperatureHeating
  3. customThe solution was decanted from the precipitated polymer
  4. stirringstirred for at least 15 minutes
  5. customAfter decanting
  6. washthe polymer was similarly washed an additional 3 times with isopropanol
  7. customThe washed polymer was dried in a forced-air oven at 70° C.
  8. customto afford 68.2 g

Quellen und Nachweise

ORD-Eintrag
ord-4719a7d9b6ef42bbaea3da68a6121075
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06299868B1

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