반응 #55044

ord-0a7595069a4a41deb8098a36b574e128

반응 조건

온도
-10°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출The free base is extracted with 1,1'-oxybisethane
  2. 2
    기타The extract is dried
  3. 3
    기타evaporated
  4. 4
    workup.DISSOLUTIONThe oily residue is dissolved in 56 parts of hexane
  5. 5
    기타the solid free base is precipitated
  6. 6
    여과It is filtered off
  7. 7
    기타dried

실험 절차

From an aqueous solution of 2.8 parts of N-(2,6-dimethylphenyl)-N-(1-propyl-4-piperidinyl)-2-thiopheneacetamide dihydrochloride, the free base is liberated by alkalization with sodium hydrogen carbonate solution. The free base is extracted with 1,1'-oxybisethane. The extract is dried and evaporated. The oily residue is dissolved in 56 parts of hexane and after cooling to -10° C., the solid free base is precipitated. It is filtered off and dried, yielding 1.6 parts of N-(2,6-dimethylphenyl)-N-(1-propyl-4-piperidinyl)-2-thiopheneacetamide; mp. 62.5° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04151286uspto-grants-1979_04