تفاعل #1904032

ord-5841f21f61df437987ab149fcc5db054

معادلة التفاعل

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
المردود 50.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرى3 bar, 100° C.
  2. 2
    ترشيحThe reaction mixture was filtered
  3. 3
    غسيلthe filtrate was washed with methanol
  4. 4
    أخرىThe combined organic phase was evaporated
  5. 5
    workup.DISTILLATIONthe residue was distilled under vacuum (1×10−2, 110° C.)

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07597875B2uspto-grants-2009_10