Reaktion #56440

Reaktionsgleichung

2-bromopropane

4-(methoxymethyl)-N-phenyl-4-piperidinamine

N,N-diethylethanamine

→

4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine

Ausbeute 42.6%

Lösungsmittel

N,N-dimethylacetamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 10.25 hours
2. 2
   TemperaturAfter cooling
3. 3
   Filtrationthe formed N,N-diethylethanamine hydrobromide is filtered off
4. 4
   workup.ADDITIONthe filtrate is diluted with water
5. 5
   ExtraktionThe product is extracted with methylbenzene
6. 6
   WaschenThe extract is washed thoroughly with water
7. 7
   Sonstigedried
8. 8
   Filtrationfiltered
9. 9
   Sonstigeevaporated
10. 10
    SonstigeThe residue is purified by column-chromatography over silica gel using
11. 11
    workup.ADDITIONa mixture of trichloromethane and methanol (90:10) as eluent
12. 12
    SonstigeThe pure fractions are collected
13. 13
    Sonstigethe eluent is evaporated

Vorschrift

A mixture of 10 parts of 2-bromopropane, 9 parts of 4-(methoxymethyl)-N-phenyl-4-piperidinamine, 4.9 parts of N,N-diethylethanamine and 72 parts of N,N-dimethylacetamide is stirred and refluxed for 10.25 hours. After cooling, the formed N,N-diethylethanamine hydrobromide is filtered off and the filtrate is diluted with water. The product is extracted with methylbenzene. The extract is washed thoroughly with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 5.7 parts (42.6%) of 4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine as an oily residue.

Quelle