반응 #1550085

반응 방정식

(R)(+)-1-(3-benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic acid dicyclohexylamine salt

hydrogen chloride

propanol

→

(R)(+)-1-(3-Benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic Acid

용매

2-propanol

반응 조건

후처리

1. 1
   온도this mixture was cooled to 5°
2. 2
   여과The resulting dicyclohexylamine hydrochloride was filtered
3. 3
   세척washed twice with 2-propanol
4. 4
   농축The combined filtrate and washings were concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue was dissolved in ether (30 ml)
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   온도This residue in 2-propanol (25 ml) was cooled to 5°
9. 9
   여과The product was collected by filtration
10. 10
    세척washed with 2-propanol

실험 절차

The (R)(+)-1-(3-benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic acid dicyclohexylamine salt thus obtained (4.1 g) was suspended in 2-propanol (25 ml) and this mixture was cooled to 5° and treated with a solution of dry hydrogen chloride in 2 propanol unit pH 2. The resulting dicyclohexylamine hydrochloride was filtered and washed twice with 2-propanol. The combined filtrate and washings were concentrated under reduced pressure. The residue was dissolved in ether (30 ml) and filtered and evaporated. This residue in 2-propanol (25 ml) was cooled to 5° and the pH adjusted to 6-7 with 2% sodium hydroxide in ethanol. The product was collected by filtration, washed with 2-propanol, and then ether. The yield of (R)(+)-1-(3-benzoylthio-1-oxopropyl)-1,2,3,4-tetrahydro-2-quinolinecarboxylic acid sodium salt was 2.0 g, m.p. 140°-144°, [α]D20 +221.3° (c 1, methanol).

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