Reaktion #1904032

Reaktionsgleichung

1,1,1-tris[2(p-methoxybenzylamino)ethyl]methane

→

1,1,1-tris(2-aminoethyl)methane

Ausbeute 50.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige3 bar, 100° C.
2. 2
   FiltrationThe reaction mixture was filtered
3. 3
   Waschenthe filtrate was washed with methanol
4. 4
   SonstigeThe combined organic phase was evaporated
5. 5
   workup.DISTILLATIONthe residue was distilled under vacuum (1×10−2, 110° C.)

Vorschrift

1,1,1-tris[2(p-methoxybenzylamino)ethyl]methane (20.0 gram, 0.036 mol) was dissolved in methanol (100 ml) and Pd(OH)2 (5.0 gram) was added. The mixture was hydrogenated (3 bar, 100° C., in an autoclave) and stirred for 5 hours. Pd(OH)2 was added in two more portions (2×5 gram) after 10 and 15 hours respectively. The reaction mixture was filtered and the filtrate was washed with methanol. The combined organic phase was evaporated and the residue was distilled under vacuum (1×10−2, 110° C.) to give 2.60 gram (50%) of 1,1,1-tris(2-aminoethyl)methane identical with the previously described Example 1.

Quelle