Реакция #1904032

ord-5841f21f61df437987ab149fcc5db054

Уравнение реакции

COc1ccc(CNCCC(CCNCc2ccc(OC)cc2)CCNCc2ccc(OC)cc2)cc1
1,1,1-tris[2(p-methoxybenzylamino)ethyl]methane
NCCC(CCN)CCN
1,1,1-tris(2-aminoethyl)methane
Выход 50.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другое3 bar, 100° C.
  2. 2
    ФильтрацияThe reaction mixture was filtered
  3. 3
    Промывкаthe filtrate was washed with methanol
  4. 4
    ДругоеThe combined organic phase was evaporated
  5. 5
    workup.DISTILLATIONthe residue was distilled under vacuum (1×10−2, 110° C.)

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07597875B2uspto-grants-2009_10