Reaktion #320603

Reaktionsgleichung

tris-(2-aminoethyl)-amine

methyl acrylate

→

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

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe batch is stirred under argon atmosphere for 5 days at room temperature and for 2 days at 50° C
2. 2
   EinengenThen, it is concentrated by evaporation in a vacuum and excess methyl acrylate
3. 3
   Sonstigeis removed by azeotropic distillation with toluene
4. 4
   Sonstige30 ml of diethyl ether, absorptively precipitated with 150 ml of hexane
5. 5
   Sonstigeafter separation of the hexane phase
6. 6
   Einengenconcentrated by evaporation in a vacuum
7. 7
   SonstigeThe product is obtained as yellowish liquid, which
8. 8
   Sonstigeis further reacted without purification

Vorschrift

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.

Quelle