反应 #1904032

反应方程式

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

→

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

收率 50.0%

溶剂

methanol

反应条件

后处理

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

实验过程

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.

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