반응 #1550084

ord-b17dbf722d34426ea3f13dafc9ff6d5b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도with cooling in an ice bath
  2. 2
    여과The resulting dicyclohexylamine hydrochloride was filtered
  3. 3
    세척washed twice with 2-propanol (20 ml)
  4. 4
    농축The combined filtrate and washings were concentrated under reduced pressure
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in ether (300 ml)
  6. 6
    건조this solution was dried over sodium sulfate
  7. 7
    농축concentrated under reduced pressure

실험 절차

The (±)-1-(3-benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic acid dicyclohexylamine salt thus obtained (35.6 g) was suspended in 2-propanol (200 ml) and this mixture was treated with a solution of dry hydrogen chloride in 2-propanol (27 ml) with cooling in an ice bath. The resulting dicyclohexylamine hydrochloride was filtered and washed twice with 2-propanol (20 ml). The combined filtrate and washings were concentrated under reduced pressure. The residue was dissolved in ether (300 ml) and this solution was dried over sodium sulfate and concentrated under reduced pressure to give 23.6 g of (±)-1-(3-benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic acid, m.p. 99°-101°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04461896uspto-grants-1984_07