반응 #56425

ord-bd0f204d655b49bc89bebaccd7c04c7b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    온도refluxed for 20 hours
  3. 3
    workup.STIRRINGstirring
  4. 4
    온도refluxing
  5. 5
    온도The reaction mixture is cooled
  6. 6
    여과filtered
  7. 7
    기타the filtrate is evaporated
  8. 8
    여과The precipitated solid salt is filtered off
  9. 9
    기타crystallized from a mixture of 2-propanone and 2-propanol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04225606uspto-grants-1980_09