Reaktion #2302549

Reaktionsgleichung

bis-(2-methyl-2-nitropropyl)amine

→

bis-(2-methyl-2-amino-propyl)amine

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe autoclave is closed
2. 2
   Sonstigepurged with nitrogen
3. 3
   workup.ADDITIONThen, hydrogen is added until the hydrogen pressure
4. 4
   Temperatursubsequently, the reaction mixture is heated to 50° C. at the same pressure
5. 5
   SonstigeThe catalyst is then separated off by filtration
6. 6
   workup.DISTILLATIONthe mixture is distilled under vacuum (100° C./33.3 mbar)
7. 7
   SonstigeA colourless oil is recovered (Boiling point: 110° C./5 mbar)

Vorschrift

490 g (2.23 mol) of bis-(2-methyl-2-nitropropyl)amine from reaction 1) are dissolved in 1200 ml of methanol and transferred into an autoclave. 60 g of Raney Ni are added. The autoclave is closed and purged with nitrogen. Then, hydrogen is added until the hydrogen pressure is 50 bars. That pressure is maintained at room temperature for 8 hours and, subsequently, the reaction mixture is heated to 50° C. at the same pressure. The catalyst is then separated off by filtration and the mixture is distilled under vacuum (100° C./33.3 mbar). A colourless oil is recovered (Boiling point: 110° C./5 mbar).

Quelle