반응 #1550084
ord-b17dbf722d34426ea3f13dafc9ff6d5b
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도with cooling in an ice bath
- 2여과The resulting dicyclohexylamine hydrochloride was filtered
- 3세척washed twice with 2-propanol (20 ml)
- 4농축The combined filtrate and washings were concentrated under reduced pressure
- 5workup.DISSOLUTIONThe residue was dissolved in ether (300 ml)
- 6건조this solution was dried over sodium sulfate
- 7농축concentrated 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°.