Réaction #56428

Équation de réaction

1-iodopropane

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

sodium carbonate

potassium iodide

1-iodopropane

→

4-chloro-N-(4-chlorophenyl)-N-(1-propyl-4-piperidinyl)benzeneacetamide

Solvants

butanol

Conditions de réaction

Traitement

1. 1
   Températurerefluxing
2. 2
   workup.STIRRINGthe whole is stirred
3. 3
   Températurerefluxed for 22 hours
4. 4
   workup.STIRRINGstirring
5. 5
   Températurerefluxing
6. 6
   TempératureThe reaction mixture is cooled
7. 7
   Filtrationfiltered
8. 8
   Autrethe filtrate is evaporated
9. 9
   workup.DISSOLUTIONThe semi-solid residue is dissolved in methylbenzene
10. 10
    FiltrationThe solution is filtered from some impurities
11. 11
    Autrethe filtrate is evaporated again
12. 12
    AutreThe residue is crystallized from 1,1'-oxybisethane at -10° C.

Mode opératoire

To a stirred and refluxing mixture of 5 parts of 4-chloro-N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, 0.4 parts of potassium iodide and 200 parts of butanol is added 4.7 parts of 1-iodopropane and the whole is stirred and refluxed for 22 hours. Then a second portion of 4.5 parts of 1-iodopropane is added and stirring and refluxing is continued for 27 h.30. The reaction mixture is cooled, filtered and the filtrate is evaporated. The semi-solid residue is dissolved in methylbenzene. The solution is filtered from some impurities and the filtrate is evaporated again. The residue is crystallized from 1,1'-oxybisethane at -10° C., yielding 0.9 parts of 4-chloro-N-(4-chlorophenyl)-N-(1-propyl-4-piperidinyl)benzeneacetamide; mp. 118.6° C.

Source