반응 #1992863

ord-7ce919abb47847c9b2927fe6893466e2

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed overnight
  2. 2
    여과filtered
  3. 3
    기타Collected solid
  4. 4
    workup.DISSOLUTIONis dissolved in hot ethanol
  5. 5
    workup.ADDITIONtreated with decolorizing charcoal
  6. 6
    농축concentrated to a smaller volume
  7. 7
    기타is recrystallized from ethanol
  8. 8
    workup.ADDITIONcontaining hydrogen chloride

실험 절차

A mixture of 1.37 g of p-chlorophenylhydrazine and 2.4 g of ethyl 4-chloro-6-methyl-5,6,7,8-tetrahydroquinoline-3-carboxylate in 75 mL of xylene is stirred and refluxed overnight, then cooled to room temperature and filtered. Collected solid is dissolved in hot ethanol, treated with decolorizing charcoal, and concentrated to a smaller volume to deposit a solid, which is recrystallized from ethanol containing hydrogen chloride to yield 2-p-chlorophenyl-2,3,6,7,8,9-hexahydro-8-methylpyrazolo[4,3-c]quinolin-3(5H)-one hydrochloride, m.p. 331°-333°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04647566uspto-grants-1987_03