반응 #1904032

반응 방정식

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

→

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

수율 50.0%

용매

methanol

반응 조건

후처리

1. 1
   기타3 bar, 100° C.
2. 2
   여과The reaction mixture was filtered
3. 3
   세척the filtrate was washed with methanol
4. 4
   기타The combined organic phase was evaporated
5. 5
   workup.DISTILLATIONthe residue was distilled under vacuum (1×10−2, 110° C.)

실험 절차

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.

출처