반응 #736781

ord-328973a2399e4ce58ec76e3303e23bf8

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed overnight
  2. 2
    기타The reaction mixture is evaporated
  3. 3
    workup.ADDITIONthe residue is treated with Et2O and 2N NaOH
  4. 4
    기타The alkaline layer is separated
  5. 5
    기타the resulting precipitate is collected
  6. 6
    세척This material is washed with EtH/Et2O
  7. 7
    기타air-dried

실험 절차

A solution of ethyl 6-benzyloxy-4-chloro-6-methyl-5,6,7,8-tetrahydroquinoline-3-carboxylate (5.0 g) and p-chlorophenylhydrazine (2.0 g) in 75 mL of n-butanol is stirred at room temperature for 4 hours, then refluxed overnight. The reaction mixture is evaporated and the residue is treated with Et2O and 2N NaOH. The alkaline layer is separated, the pH is adjusted at 8 with dilute HCl, and the resulting precipitate is collected. This material is washed with EtH/Et2O and air-dried to obtain 8-benzyloxy-2-p-chlorophenyl-8-methyl-2,3,6,7,8,9-hexahydropyrazolo[4,3-c]quinolin-3(5H)-one.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04740512uspto-grants-1988_04