Methyl Acrylate → Tris-[N,N-bis-(methoxycarbonylethyl)-2-aminoethyl]-amine

HRID 233421Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 233421
[NH2:1][CH2:2][CH2:3][N:4]([CH2:8][CH2:9][NH2:10])[CH2:5][CH2:6][NH2:7].[C:11]([O:15][CH3:16])(=[O:14])[CH:12]=[CH2:13]>CO>[CH3:16][O:15][C:11]([CH2:12][CH2:13][N:1]([CH2:13][CH2:12][C:11]([O:15][CH3:16])=[O:14])[CH2:2][CH2:3][N:4]([CH2:8][CH2:9][N:10]([CH2:13][CH2:12][C:11]([O:15][CH3:16])=[O:14])[CH2:13][CH2:12][C:11]([O:15][CH3:16])=[O:14])[CH2:5][CH2:6][N:7]([CH2:13][CH2:12][C:11]([O:15][CH3:16])=[O:14])[CH2:13][CH2:12][C:11]([O:15][CH3:16])=[O:14])=[O:14]

Komponenten

4

Edukt 2

HCID 7294Methyl AcrylateHCID 77731Tris(2-aminoethyl)amine

Produkt 1

HCID 53701481Tris-[N,N-bis-(methoxycarbonylethyl)-2-aminoethyl]-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

14.69 g (0.100 mol) of tris-(2-aminoethyl)-amine, dissolved in 20 ml of methanol, is instilled in 103.3 g (1.20 mol) of methyl acrylate with stirring at 20° C. The batch is stirred under argon atmosphere for 5 days at room temperature and for 2 days at 50° C. Then, it is concentrated by evaporation in a vacuum and excess methyl acrylate is removed by azeotropic distillation with toluene. The residue is taken up in 150 ml of methanol and 30 ml of diethyl ether, absorptively precipitated with 150 ml of hexane and, after separation of the hexane phase, concentrated by evaporation in a vacuum. The product is obtained as yellowish liquid, which is further reacted without purification.

Aufarbeitung

  1. stirringThe batch is stirred under argon atmosphere for 5 days at room temperature and for 2 days at 50° C
  2. concentrationThen, it is concentrated by evaporation in a vacuum and excess methyl acrylate
  3. customis removed by azeotropic distillation with toluene
  4. custom30 ml of diethyl ether, absorptively precipitated with 150 ml of hexane
  5. customafter separation of the hexane phase
  6. concentrationconcentrated by evaporation in a vacuum
  7. customThe product is obtained as yellowish liquid, which
  8. customis further reacted without purification

Quellen und Nachweise

ORD-Eintrag
ord-3151e6f1b36049afa74cac711ee48f42
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05593660

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