反応 #1904032

反応方程式

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

→

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

収率 50.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他3 bar, 100° C.
2. 2
   ろ過The reaction mixture was filtered
3. 3
   洗浄the filtrate was washed with methanol
4. 4
   その他The combined organic phase was evaporated
5. 5
   workup.DISTILLATIONthe residue was distilled under vacuum (1×10−2, 110° C.)

実験手順

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.

出典