반응 #155360

ord-36d795d1da95405ea6c75daa91c54980

반응 방정식

Cc1cc(NCCCN(C)CCCNc2ccc([N+](=O)[O-])c(C)c2)ccc1[N+](=O)[O-]
N1-Methyl-N3-(3-methyl-4-nitrophenyl)-N1-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1,3-propanediamine
C=CCOS(=O)(=O)c1ccc(C)cc1
allyl p-toluene sulfonate
Cc1ccccc1
toluene
C=CC[N+](C)(CCCNc1ccc([N+](=O)[O-])c(C)c1)CCCNc1ccc([N+](=O)[O-])c(C)c1.Cc1ccc(S(=O)(=O)[O-])cc1
product
C=CC[N+](C)(CCCNc1ccc([N+](=O)[O-])c(C)c1)CCCNc1ccc([N+](=O)[O-])c(C)c1.Cc1ccc(S(=O)(=O)[O-])cc1
N-allyl-N-methyl-3-[(3-methyl-4-nitrophenyl)amino]-N-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1-propanaminium p-toluene sulfonate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타separated out in the form of an oily substance
  2. 2
    기타This oil was separated from the supernatant liquid
  3. 3
    기타by decanting
  4. 4
    기타dried
  5. 5
    온도On further cooling the oil
  6. 6
    기타after drying could
  7. 7
    기타be crushed

실험 절차

N1-Methyl-N3-(3-methyl-4-nitrophenyl)-N1-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1,3-propanediamine (60.2 g, 0.14 mol) from step 7.1 was heated under reflux with allyl p-toluene sulfonate (34.0 g, 0.16 mol) in 500 ml toluene for 6 hours. As the reaction progressed the product separated out in the form of an oily substance. This oil was separated from the supernatant liquid by decanting and dried. On further cooling the oil initially solidified to a glassy material and after drying could be crushed to afford the product as a brown powder. Yield: 66.0 g (72.5%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08821592B1uspto-grants-2014_09