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Hydrochloric Acid → HCID 3032237, Verbindung

HRID 1462902
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1462902
C1(NC2CCCCC2)CCCCC1.[C:14]([S:22][CH2:23][CH2:24][C:25]([N:27]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH2:30][CH2:29][CH:28]1[C:37]([OH:39])=[O:38])=[O:26])(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.Cl>CC(O)C>[C:14]([S:22][CH2:23][CH2:24][C:25]([N:27]1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH2:30][CH2:29][CH:28]1[C:37]([OH:39])=[O:38])=[O:26])(=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 86739569HCID 86739569, Verbindung

Produkt 1

HCID 3032237HCID 3032237, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel2×

Versuchsvorschrift

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°.

Aufarbeitung

  1. temperaturewith cooling in an ice bath
  2. filtrationThe resulting dicyclohexylamine hydrochloride was filtered
  3. washwashed twice with 2-propanol (20 ml)
  4. concentrationThe combined filtrate and washings were concentrated under reduced pressure
  5. dissolutionThe residue was dissolved in ether (300 ml)
  6. dry with materialthis solution was dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b17dbf722d34426ea3f13dafc9ff6d5b
Quelldatensatz
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04461896

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