HCID 19968441, Verbindung → HCID 11779419, Verbindung

HRID 975829Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 975829
S(O)(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1>[OH-].[Na+]>[ClH:6].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1

Komponenten

3

Edukt 1

HCID 19968441HCID 19968441, Verbindung

Produkt 1

HCID 11779419HCID 11779419, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

A suspension of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene sulphate (13 g prepared in a similar manner to that described in Example 5) in 1M aqueous sodium hydroxide solution (200 ml) was stirred at ambient temperature for 1 hour, then the free base was extracted into ether (3×150 ml). The extracts were combined, dried over magnesium sulphate, concentrated to a volume of 150 ml, and filtered. The filtrate was cooled in ice and saturated with hydrogen chloride. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours and at 60° C. for 8 hours to give 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene hydrochloride as a white solid. Yield 8.6 g, mp >300° C.

Aufarbeitung

  1. customprepared in a similar manner to that
  2. extractionthe free base was extracted into ether (3×150 ml)
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated to a volume of 150 ml
  5. filtrationfiltered
  6. temperatureThe filtrate was cooled in ice and saturated with hydrogen chloride
  7. filtrationThe resulting solid was collected by filtration
  8. washwashed with ether
  9. customdried in vacuo at ambient temperature for 24 hours and at 60° C. for 8 hours

Quellen und Nachweise

ORD-Eintrag
ord-de1eb73209b64ad9adec0142c9690f70
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05610161

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