Reaktion #155360

Reaktionsgleichung

N1-Methyl-N3-(3-methyl-4-nitrophenyl)-N1-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1,3-propanediamine

allyl p-toluene sulfonate

toluene

→

product

N-allyl-N-methyl-3-[(3-methyl-4-nitrophenyl)amino]-N-{3-[(3-methyl-4-nitrophenyl)amino]propyl}-1-propanaminium p-toluene sulfonate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeseparated out in the form of an oily substance
2. 2
   SonstigeThis oil was separated from the supernatant liquid
3. 3
   Sonstigeby decanting
4. 4
   Sonstigedried
5. 5
   TemperaturOn further cooling the oil
6. 6
   Sonstigeafter drying could
7. 7
   Sonstigebe crushed

Vorschrift

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%).

Quelle