Reaktion #55032

Reaktionsgleichung

2-bromopropane

N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide

sodium carbonate

potassium iodide

2-bromopropane

→

N-(4-chlorophenyl)-N-[1-(1-methylethyl)-4-piperidinyl]benzeneacetamide hydrochloride

Lösungsmittel

2-propanone

butanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   Temperaturrefluxed for 20 hours
3. 3
   workup.STIRRINGstirring
4. 4
   Temperaturrefluxing
5. 5
   TemperaturThe reaction mixture is cooled
6. 6
   Filtrationfiltered
7. 7
   Sonstigethe filtrate is evaporated
8. 8
   FiltrationThe precipitated solid salt is filtered off
9. 9
   Sonstigecrystallized from a mixture of 2-propanone and 2-propanol

Vorschrift

To a stirred suspension of 5 parts of N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, a few crystals of potassium iodide in 200 parts of butanol is added dropwise 4 parts of 2-bromopropane at room temperature. After the addition is complete, the whole is stirred and refluxed for 20 hours. Then the second portion of 4 parts of 2-bromopropane is added and stirring and refluxing is continued for another 19 hours. The reaction mixture is cooled, filtered and the filtrate is evaporated. From the oily free base, the hydrochloride salt is prepared in the conventional manner in 1,1'-oxybisethane and 2-propanone. The precipitated solid salt is filtered off and crystallized from a mixture of 2-propanone and 2-propanol, yielding 2 parts of N-(4-chlorophenyl)-N-[1-(1-methylethyl)-4-piperidinyl]benzeneacetamide hydrochloride; mp. 263° C.

Quelle